megalomania
October 7th, 2002, 02:58 PM
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted December 21, 2000 08:22 PM
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I tried AP yesterday, using Megolamania's recipe on his explosives page, but cut it in half. I did two batches, the first using 1.5mL of acid and the other I kept at 3mL. The acid I used was 75% Phosporic Acid. The hydrogen peroxide is 3% CVS brand (yes I did use 10x the req'd volume, which would be 150mL, since the recipe was cut 50%).
When I was adding the acid, the area the drops went in, would cloud up, then clear. By the time I added all the acid the mixture was a little cloudy. After 3hrs, the solution was very cloudy and I saw no crystals. I did keep the container covered loosely with a piece of cardboard, the jars were set outside out of the wind, the cover to prevent contamination.
After 5hrs I still had nothing. So I decided to try again using the same recipe with the original amounts. After 12hrs in the first two batches and 7hrs in the second I could still smell acetone, so I decided to evaporate some with moving air. I evaporated 2mL of solution from one of the first batches. Remaining was a minute amount of pasty crystals. I let them set for about an hour and held a match to them, nothing happened.
It's been over 24hrs for each batch now and I just filtered the full recipe solution, thinking maybe it's so cloudy I can't see anything. Nothing ended up on the filter paper. So I have 3 glass jars full of a cloudy mixture, the smell of acetone is still evident, though not as much from when I started, except for the full recipe batch, in which the smell is still pretty strong.
Am I doing anything wrong and any suggestions?
CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted December 21, 2000 09:11 PM
--------------------------------------------------------------------------------
Phosphoric acid may not be strong enough to be a sufficient catalyst to produce AP in 24 hours. wait like 48 and see what happens. i would suggest you use 32% HCl, i know a kid who uses this and it works fine.
------------------
...Æ
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted December 21, 2000 09:51 PM
--------------------------------------------------------------------------------
Will do
I put some of the solution in a water bath to rid any excess acetone. AP is soluble in Acetone right?
I kinda rushed it though, I was outside and thought what the heck, I didn't expect much yield anyhow. So I let the acetone boil and used a large enough beaker to get somewhat of a reflux. After the first boiling range I let the mixture cool down to about room temp. I then put the jar in a ice-salt bath. I then using a pipette transferred 10mL of the solution to an ice bath, hoping for a precipitate. In either case I got nothing. I have more material sitting outside, will wait and see what it looks like tomorrow.
I'm assuming sense it is said that most acids will work that it is H+ that is the catalyst?
Lost
Frequent Poster
Posts: 89
From:
Registered: SEP 2000
posted December 22, 2000 05:55 AM
--------------------------------------------------------------------------------
Yes, AP is soluble in acetone. Any mineral acid will work, stay away from organic ones though...
------------------
-Lost
<a href="http://www.noneinc.org" target="_blank">http://www.noneinc.org</a>
SofaKing
Frequent Poster
Posts: 392
From: YEAH RIGHT !!
Registered: SEP 2000
posted December 22, 2000 09:55 AM
--------------------------------------------------------------------------------
Sounds like you didn't cool the reaction properly. You must cool during the entire reaction. Also have some pateince, using 3% peroxide takes three days, and with such a small batch will give little results.
Arthis
Frequent Poster
Posts: 203
From:
Registered: OCT 2000
posted December 22, 2000 11:50 AM
--------------------------------------------------------------------------------
I know someone who has a dog whose mother was the dog of a man whose pastor had a friend whose wife had an uncle who had a son who had a friend who had a friend who had tried to do it with sulfuric acid, and it worked (acording to the father of a friend who knew the wife of the pastor who knew the father of the friend who knew that guy)...
In low conc., it may not work well, as in low quantities, and may take much time. Just let it for a few days outside, and it should work a little.
BoB-
Frequent Poster
Posts: 649
From:
Registered: SEP 2000
posted December 22, 2000 05:57 PM
--------------------------------------------------------------------------------
Damn Arthis, your connected.
Some acids just suck donkey's when it comes to use as a catalyst in the AP procedure.
Keep the solution cold to prevent the dimer from forming.
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 02, 2001 10:48 PM
--------------------------------------------------------------------------------
I tried to make AP again with 3%H2O2, instead of phosphoric acid I used sulfuric. I used 300mL 3%H2O2, 3mL H2SO4, and 50mL of acetone. My glass jar set in an unheated garage for a few hours short of one week. The outside temps never rose above freezing nor did the garage.
I can't make out the smell of acetone anymore, but more of a acidic musty odor. The solution is cloudy, but I don't see any crystals.
The sulfuric acid I used is not pure and I'm not sure the concentration. It's actually the quickest source I had, which was a trip to the local hardware store. It's non fuming and it's sold as drain opener, called liquid fire. I'm sure it has some additives as it's fairly viscous (probably ~600cPs)and a deep purple color.
So is it the acid again? Should I flash off the liquid? It'll be another week before I'll be able to do anything with the liquid, whatever the heck is in it.
I do now have H2SO4, 98% by weight, but plan on obtainging 30% H2O2 b4 I try again.
I feel like a real idiot here, what the hell am I doing wrong? I use a graduated cylinder to measure out everything, use clean glassware, and cover with parafilm to prevent contamination. I'm also positive that the solution never once was exposed to temps above 5°C, I chilled all ingredients and glass ware.
Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted January 03, 2001 07:47 AM
--------------------------------------------------------------------------------
The problem may be in that you've cooled it too well! Some lab procedures for making AP suggest you heat the reactant vessels with a bunsen to get the reaction going. I and some ffriends have found that you can "kick start" reluctant AP batches by adding 30-50ml extra acid at once, I guess the heating (un-noticable) is what gets it going.
I too used H2SO4 drain cleaner for my last batch (viscous and purple) and had problems with cloudiness, AP non-appearance etc. I'm switching back to 32% Hcl!
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 03, 2001 06:29 PM
--------------------------------------------------------------------------------
Thanks, what is your exact procedure, if you don't mind. Do you heat or use extra acid?
Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted January 04, 2001 05:28 PM
--------------------------------------------------------------------------------
I use equal parts of 6% h2o2 and nail varnish remover (practically poure acetone), I mix the two in a jar in an ice bath and leave it to chill, I then add 3ml of 32% hcl and stir for two minutes (I add the acid drop by drop over the whole two minutes), I keep adding 3ml hcl untill I've added 15ml in total, I usually continue string for a few more minutes. I leave the jar in the ice bath and leave it for three days. Obviously the ice melts, but by then the reaction is over and the water keeps it reasonably cool. I find that if I do a batch in the morning, by night time the solution is still perfectly clear, then in the next moring all these cyrstals have appeared!
The crystals are usually flaky like snowflakes, but one time I used 18% h2o2 and got giant (upto 1") needles.
I did a rush batch once, I threw all the chemicals into a jar and stuck it into the fridge. Crystals appeared more quickly but it was a very fine powder and I didn't get as good a yeild. Course crystals are easier to wash as you can blast them with water without fear of them escaping through the filter cloth.
I will try Sofaking's suggested ratios soon with much less acetone, because if AP is soluble in acetone then some of the batch could be "trapped" in the solution.
BTW, I've never had any problems with AP not appearing using HCl, the solution is allways very clear with a layer of crystals on the bottom of the jar and a thinner layer on the surface.
I think that's about it!
[This message has been edited by Anthony (edited January 04, 2001).]
SafetyLast
Frequent Poster
Posts: 232
From: the cretaceous period
Registered: OCT 2000
posted January 04, 2001 09:04 PM
--------------------------------------------------------------------------------
I always use 2 cups of 3% H2O2, 1/2cup of nail polish remover that is pure acetone (yup same conc. as the stuff in the metal cans but costs less and says 100%pure) and 1/2-1 cup of 32% HCl I use a quart sized canning jar and I put it in a cooler with
6-8 cups of Ice.
I add more ice every 6-10 hours and I monitor the temp of the bath and make sure it stays about 38-42 degrees Farenheight for 60 hours and then I filter it using a couple coffee filters. I wash it under tap water (set faucet on low)
I scrape the wet powder onto a piece of contruction paper and let it dry for 10 hours on my bookshelf
I haven't had any problems storing small ammounts of powder (about 5-10 grams) in the open air for a few days.
I was just wondering if it is possible to add to much acid and how long can you store the powder in open air?
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 05, 2001 11:23 PM
--------------------------------------------------------------------------------
Maybe it didn't fail this go around. I just had a friend check out a jar I left set. He said there were quite a few crystals on top and some on the bottom. I can't wait to "play". He estimated that maybe there was 100g, but he's new to such things so I'm not sure. He's gonna leave it alone till I get over there next week. Sweet. It took 2 weeks though.
I did get some 50% w/w Hydrochloric acid that I'll cut to 32%. And have another go at it.
Thanks for all the help.
CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted January 06, 2001 12:01 AM
--------------------------------------------------------------------------------
i have always heard of kids using 32% concentration HCl and they have never had any problems. the ratios they use go something like this. 2 cups 3% H2O2, 1 cup acetone, and about half a cup of 32% HCl. this is then set in a cool place to let the reaction complete. within 48 hours all crystals that are to be made, have been made. (like you mentioned, The Real, some crystals on top, most on bottem with a few suspended in the middle.) The way these chemicals are mixed (in a glass jar) is as follows: the 2 cups H2O2 is put in the jar followed by the 1 cup of acetone. the half cup of HCl is just dumped in all at once, the mixture gets noticably warm (but not toowarm mind you, just noticable) this method produces very fine AP crystals. the amount attained, when the AP compresses itself due to its own weight, is a little less than a cup of actual AP (maybe a cup). this is a good yield i would say. pretty economical in my view also.
as for the person who said you might have chilled the reaction too much, i don't think this is possible. i have personnaly seen ice chuncks form in the mixture because the mix was left next to an open window in the winter. this did not appear to harm the reaction at all. as for the H+ ions being the actual catalyst, i think this is correct.
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted December 21, 2000 08:22 PM
--------------------------------------------------------------------------------
I tried AP yesterday, using Megolamania's recipe on his explosives page, but cut it in half. I did two batches, the first using 1.5mL of acid and the other I kept at 3mL. The acid I used was 75% Phosporic Acid. The hydrogen peroxide is 3% CVS brand (yes I did use 10x the req'd volume, which would be 150mL, since the recipe was cut 50%).
When I was adding the acid, the area the drops went in, would cloud up, then clear. By the time I added all the acid the mixture was a little cloudy. After 3hrs, the solution was very cloudy and I saw no crystals. I did keep the container covered loosely with a piece of cardboard, the jars were set outside out of the wind, the cover to prevent contamination.
After 5hrs I still had nothing. So I decided to try again using the same recipe with the original amounts. After 12hrs in the first two batches and 7hrs in the second I could still smell acetone, so I decided to evaporate some with moving air. I evaporated 2mL of solution from one of the first batches. Remaining was a minute amount of pasty crystals. I let them set for about an hour and held a match to them, nothing happened.
It's been over 24hrs for each batch now and I just filtered the full recipe solution, thinking maybe it's so cloudy I can't see anything. Nothing ended up on the filter paper. So I have 3 glass jars full of a cloudy mixture, the smell of acetone is still evident, though not as much from when I started, except for the full recipe batch, in which the smell is still pretty strong.
Am I doing anything wrong and any suggestions?
CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted December 21, 2000 09:11 PM
--------------------------------------------------------------------------------
Phosphoric acid may not be strong enough to be a sufficient catalyst to produce AP in 24 hours. wait like 48 and see what happens. i would suggest you use 32% HCl, i know a kid who uses this and it works fine.
------------------
...Æ
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted December 21, 2000 09:51 PM
--------------------------------------------------------------------------------
Will do
I put some of the solution in a water bath to rid any excess acetone. AP is soluble in Acetone right?
I kinda rushed it though, I was outside and thought what the heck, I didn't expect much yield anyhow. So I let the acetone boil and used a large enough beaker to get somewhat of a reflux. After the first boiling range I let the mixture cool down to about room temp. I then put the jar in a ice-salt bath. I then using a pipette transferred 10mL of the solution to an ice bath, hoping for a precipitate. In either case I got nothing. I have more material sitting outside, will wait and see what it looks like tomorrow.
I'm assuming sense it is said that most acids will work that it is H+ that is the catalyst?
Lost
Frequent Poster
Posts: 89
From:
Registered: SEP 2000
posted December 22, 2000 05:55 AM
--------------------------------------------------------------------------------
Yes, AP is soluble in acetone. Any mineral acid will work, stay away from organic ones though...
------------------
-Lost
<a href="http://www.noneinc.org" target="_blank">http://www.noneinc.org</a>
SofaKing
Frequent Poster
Posts: 392
From: YEAH RIGHT !!
Registered: SEP 2000
posted December 22, 2000 09:55 AM
--------------------------------------------------------------------------------
Sounds like you didn't cool the reaction properly. You must cool during the entire reaction. Also have some pateince, using 3% peroxide takes three days, and with such a small batch will give little results.
Arthis
Frequent Poster
Posts: 203
From:
Registered: OCT 2000
posted December 22, 2000 11:50 AM
--------------------------------------------------------------------------------
I know someone who has a dog whose mother was the dog of a man whose pastor had a friend whose wife had an uncle who had a son who had a friend who had a friend who had tried to do it with sulfuric acid, and it worked (acording to the father of a friend who knew the wife of the pastor who knew the father of the friend who knew that guy)...
In low conc., it may not work well, as in low quantities, and may take much time. Just let it for a few days outside, and it should work a little.
BoB-
Frequent Poster
Posts: 649
From:
Registered: SEP 2000
posted December 22, 2000 05:57 PM
--------------------------------------------------------------------------------
Damn Arthis, your connected.
Some acids just suck donkey's when it comes to use as a catalyst in the AP procedure.
Keep the solution cold to prevent the dimer from forming.
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 02, 2001 10:48 PM
--------------------------------------------------------------------------------
I tried to make AP again with 3%H2O2, instead of phosphoric acid I used sulfuric. I used 300mL 3%H2O2, 3mL H2SO4, and 50mL of acetone. My glass jar set in an unheated garage for a few hours short of one week. The outside temps never rose above freezing nor did the garage.
I can't make out the smell of acetone anymore, but more of a acidic musty odor. The solution is cloudy, but I don't see any crystals.
The sulfuric acid I used is not pure and I'm not sure the concentration. It's actually the quickest source I had, which was a trip to the local hardware store. It's non fuming and it's sold as drain opener, called liquid fire. I'm sure it has some additives as it's fairly viscous (probably ~600cPs)and a deep purple color.
So is it the acid again? Should I flash off the liquid? It'll be another week before I'll be able to do anything with the liquid, whatever the heck is in it.
I do now have H2SO4, 98% by weight, but plan on obtainging 30% H2O2 b4 I try again.
I feel like a real idiot here, what the hell am I doing wrong? I use a graduated cylinder to measure out everything, use clean glassware, and cover with parafilm to prevent contamination. I'm also positive that the solution never once was exposed to temps above 5°C, I chilled all ingredients and glass ware.
Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted January 03, 2001 07:47 AM
--------------------------------------------------------------------------------
The problem may be in that you've cooled it too well! Some lab procedures for making AP suggest you heat the reactant vessels with a bunsen to get the reaction going. I and some ffriends have found that you can "kick start" reluctant AP batches by adding 30-50ml extra acid at once, I guess the heating (un-noticable) is what gets it going.
I too used H2SO4 drain cleaner for my last batch (viscous and purple) and had problems with cloudiness, AP non-appearance etc. I'm switching back to 32% Hcl!
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 03, 2001 06:29 PM
--------------------------------------------------------------------------------
Thanks, what is your exact procedure, if you don't mind. Do you heat or use extra acid?
Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted January 04, 2001 05:28 PM
--------------------------------------------------------------------------------
I use equal parts of 6% h2o2 and nail varnish remover (practically poure acetone), I mix the two in a jar in an ice bath and leave it to chill, I then add 3ml of 32% hcl and stir for two minutes (I add the acid drop by drop over the whole two minutes), I keep adding 3ml hcl untill I've added 15ml in total, I usually continue string for a few more minutes. I leave the jar in the ice bath and leave it for three days. Obviously the ice melts, but by then the reaction is over and the water keeps it reasonably cool. I find that if I do a batch in the morning, by night time the solution is still perfectly clear, then in the next moring all these cyrstals have appeared!
The crystals are usually flaky like snowflakes, but one time I used 18% h2o2 and got giant (upto 1") needles.
I did a rush batch once, I threw all the chemicals into a jar and stuck it into the fridge. Crystals appeared more quickly but it was a very fine powder and I didn't get as good a yeild. Course crystals are easier to wash as you can blast them with water without fear of them escaping through the filter cloth.
I will try Sofaking's suggested ratios soon with much less acetone, because if AP is soluble in acetone then some of the batch could be "trapped" in the solution.
BTW, I've never had any problems with AP not appearing using HCl, the solution is allways very clear with a layer of crystals on the bottom of the jar and a thinner layer on the surface.
I think that's about it!
[This message has been edited by Anthony (edited January 04, 2001).]
SafetyLast
Frequent Poster
Posts: 232
From: the cretaceous period
Registered: OCT 2000
posted January 04, 2001 09:04 PM
--------------------------------------------------------------------------------
I always use 2 cups of 3% H2O2, 1/2cup of nail polish remover that is pure acetone (yup same conc. as the stuff in the metal cans but costs less and says 100%pure) and 1/2-1 cup of 32% HCl I use a quart sized canning jar and I put it in a cooler with
6-8 cups of Ice.
I add more ice every 6-10 hours and I monitor the temp of the bath and make sure it stays about 38-42 degrees Farenheight for 60 hours and then I filter it using a couple coffee filters. I wash it under tap water (set faucet on low)
I scrape the wet powder onto a piece of contruction paper and let it dry for 10 hours on my bookshelf
I haven't had any problems storing small ammounts of powder (about 5-10 grams) in the open air for a few days.
I was just wondering if it is possible to add to much acid and how long can you store the powder in open air?
The Real
Frequent Poster
Posts: 136
From: Columbus, OH
Registered: DEC 2000
posted January 05, 2001 11:23 PM
--------------------------------------------------------------------------------
Maybe it didn't fail this go around. I just had a friend check out a jar I left set. He said there were quite a few crystals on top and some on the bottom. I can't wait to "play". He estimated that maybe there was 100g, but he's new to such things so I'm not sure. He's gonna leave it alone till I get over there next week. Sweet. It took 2 weeks though.
I did get some 50% w/w Hydrochloric acid that I'll cut to 32%. And have another go at it.
Thanks for all the help.
CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted January 06, 2001 12:01 AM
--------------------------------------------------------------------------------
i have always heard of kids using 32% concentration HCl and they have never had any problems. the ratios they use go something like this. 2 cups 3% H2O2, 1 cup acetone, and about half a cup of 32% HCl. this is then set in a cool place to let the reaction complete. within 48 hours all crystals that are to be made, have been made. (like you mentioned, The Real, some crystals on top, most on bottem with a few suspended in the middle.) The way these chemicals are mixed (in a glass jar) is as follows: the 2 cups H2O2 is put in the jar followed by the 1 cup of acetone. the half cup of HCl is just dumped in all at once, the mixture gets noticably warm (but not toowarm mind you, just noticable) this method produces very fine AP crystals. the amount attained, when the AP compresses itself due to its own weight, is a little less than a cup of actual AP (maybe a cup). this is a good yield i would say. pretty economical in my view also.
as for the person who said you might have chilled the reaction too much, i don't think this is possible. i have personnaly seen ice chuncks form in the mixture because the mix was left next to an open window in the winter. this did not appear to harm the reaction at all. as for the H+ ions being the actual catalyst, i think this is correct.