megalomania
June 21st, 2003, 05:10 PM
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 03:37 AM
--------------------------------------------------------------------------------
I have ordered a 24/40 distillation setup from UGT. I plan on making some high concentration nitric acid. But first i need to aquire a vacuum pump. I have heard things of getting these from fridges. So i can just remove the compressor out of a refrigerator and hook it up in reverse to use it as a vacuum pump to distill nitric acid (with a trap)? do you think a aspirator would be efficient to do the job instead of a pump?
I am quite confused on the subject so any input is appreciated.
------------------
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Explosives Archive
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 07:50 AM
--------------------------------------------------------------------------------
I used to have two frezzer compressors, hooked up in series backwards, that I used for all sorts of vaccuum things. They could get to less than 0.5 torr (atmospheric pressure = roughly 760). But they burnt out, so I can't use them anymore.
One freezer compressor would do very well to make HNO3, aspirators of the kind that you attach to taps also work well if the water flows fast enough. If you use a freezer compressor, be careful that your glasswear doesn't implode. I know for a fact that conical flasks do quite easily.
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 08:23 AM
--------------------------------------------------------------------------------
Wonerfull. i really dont care if it burns out after awhile because i can just look for another freezer and take it out again. i have all round bottom flasks and the setup is mabe for vacuum distillations so thres no worry about implosions. heres a pic of the setup:
http://www.unitedglasstech.com/DistillAPPARA24-40-2.jpg (or see attached)
wantsomfet
Frequent Poster
Posts: 239
From: EU
Registered: JAN 2001
posted 07-04-2001 09:02 AM
--------------------------------------------------------------------------------
Nice! Are that TEFLON fittings at the joints?
------------------
for best catfood visit:
kangaroooo.cjb.net
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 12:03 PM
--------------------------------------------------------------------------------
I use a refrigerator compressor i found at a tag sale for $35. An aspirator will work if you use one of those pool pumps to make the water flow, and it can provide a good vacuum and another plus is that you dont need a trap. Those are ground glass fittings wantsomefet, i have the same setup =). And that setup wont implode unless you nick it or force is applied, because ive been vacuum distilling HNO3 about 3 times a week since i got it (1 1/2 months ago) and its still in tip top shape.
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 12:11 PM
--------------------------------------------------------------------------------
Not a bad setup! How much is that costing ya?
I got a load of glasswear very cheap at an army surplus place a few years back. I don't know why it was there, but I got two liebigs, loads of miscellaneous flasks and beakers, connectors, stoppers, etc etc. The whole lot was quite expensive, but a fraction of the new cost.
I got half way towards making one of the condensers (2 feet long) into a CO2 laser, but then gave up. I might finish it some day, because a 200 watt CW laser would be nice to have.
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 02:31 PM
--------------------------------------------------------------------------------
This setup costs $125 US from UGT (unitedglasstech.com). Thats quite low compared to other companies who sell it for around 200 or even more.
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 02:57 PM
--------------------------------------------------------------------------------
I have been talking to some people that have distillation setups similar to mine. One person says that vauum isnt necessar. he claims that when distilled 3 times with conc. H2S04 (tritration) and treated with urea, he can get 99.362% hno3. But i still want to use a vacuum. Does anyone know what kind of tubes i should use with the vacuum?
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 03:08 PM
--------------------------------------------------------------------------------
You mean to connect the setup to the pump? You can buy vaccuum tubing from some places that sell glasswear etc, not sure of any specific sources though. A lot depends on what you can attach to the pump and distillation setup. I doubt that a very high vaccuum will be needed, so most tubes will work except soft rubber. Thin glass will work very well if you can attach it.
Although I never used to use a vaccuum to make HNO3 even when I had my pumps. Using a water bath helps to keep the reaction from overheating too much, and the product worked for RDX when decolourised. I'm going to try the Ca(NO3)2 / H2SO4 method, and filter out the CaSO4 and see if that works for RDX. Wish me luck!
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 03:18 PM
--------------------------------------------------------------------------------
Ok, and how do i use urea to perge NOx, NO2, etc? The calcium nitrate method works quite well, ive done it a few times. good luck.
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 05:11 PM
--------------------------------------------------------------------------------
I use 3/8 inch wire reinforced plastic tubing i got from my hardware store. It works really well! A vacuum isnt neccesary, that is correct, but if done correctly you can get concentrated (96%+) HNO3 from just one distillation! To purge HNO3 of urea, just add it in really small amounts until the acid is completely clear, stirring till it dissolves. It wont really polute the acid since i think a concentration higher than 80% of HNO3 will just decompose the urea, although some urea nitrate may form. You usually have to add about 1-2% by weight if your acid is NOx-heavy.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 07-04-2001 06:51 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 07:58 PM
--------------------------------------------------------------------------------
This is really interesting...especially the calcium nitrate + sulfuric method. Can anyone elaborate a bit more on that? Precise procedure? already have a good idea but not completely clear...
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 08:09 PM
--------------------------------------------------------------------------------
Its just like kno3 + h2so4 except you use calcium nitrate and it works better than kno3. There is no violent reaction that takes place either.
------------------
How much power will you lose if you do not know what they already know?
Explosives Archive
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-05-2001 03:39 AM
--------------------------------------------------------------------------------
I can get a very large compressor for large store freezers most likely now. If it's too powerful ill put a dimmer switch to turn the power down. Does anyone have any idea about what to use for traps? im thinking a water trap, then a solid trap with some sodium bicarb and some sort of very hygroscopic material to absorb some of the water. Unles someone else has a more simple plan
------------------
How much power will you lose if you do not know what they already know?
Explosives Archive
[This message has been edited by ALENGOSVIG1 (edited July 05, 2001).]
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-05-2001 07:32 AM
--------------------------------------------------------------------------------
If you can get hold of it, then surround a flask (the trap) with a slurry of dry ice and acetone. This will condense and freeze just about anything, and stop it from getting into the pump.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 07-05-2001 09:21 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Gab
New Member
Posts: 16
From: Québec, Canada
Registered: MAR 2001
posted 07-05-2001 10:26 AM
--------------------------------------------------------------------------------
I have found this picture. It looks like a rather cheap vacuum.
http://www.geocities.com/CapeCanaveral/Lab/4256/2.jpg
[This message has been edited by Gab (edited July 05, 2001).]
SawedOff8gaugeman
Frequent Poster
Posts: 56
From: Finland
Registered: JUN 2001
posted 07-06-2001 04:01 PM
--------------------------------------------------------------------------------
quote:
--------------------------------------------------------------------------------
Originally posted by Mr Cool:
I got half way towards making one of the condensers (2 feet long) into a CO2 laser, but then gave up. I might finish it some day, because a 200 watt CW laser would be nice to have.
--------------------------------------------------------------------------------
Sounds cool!
(This is off-topic ) I would like to know "how to", can you possibly point me to some site or something ??
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-06-2001 04:08 PM
--------------------------------------------------------------------------------
I'll e-mail you some stuff on CO2 and other high-power lasers (nitrogen and dye are easy to make.) If anyone else would like some info just ask here.
I made a flashlamp pumped dye laser, and first I used cheap first-surface mirrors. The Al coating on them was almost totally vapourised on the first shot! So I had to pay for better ones. Also the flash lamps exploded every 50 shots or so, because I was putting way too much energy into them. So it all became rather expensive. I'll have to find a way to make my own high-power flash lamps, and start using it again because they're quite fun if you like that sort of thing.
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 03:37 AM
--------------------------------------------------------------------------------
I have ordered a 24/40 distillation setup from UGT. I plan on making some high concentration nitric acid. But first i need to aquire a vacuum pump. I have heard things of getting these from fridges. So i can just remove the compressor out of a refrigerator and hook it up in reverse to use it as a vacuum pump to distill nitric acid (with a trap)? do you think a aspirator would be efficient to do the job instead of a pump?
I am quite confused on the subject so any input is appreciated.
------------------
How much power will you lose if you do not know what they already know?
Explosives Archive
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 07:50 AM
--------------------------------------------------------------------------------
I used to have two frezzer compressors, hooked up in series backwards, that I used for all sorts of vaccuum things. They could get to less than 0.5 torr (atmospheric pressure = roughly 760). But they burnt out, so I can't use them anymore.
One freezer compressor would do very well to make HNO3, aspirators of the kind that you attach to taps also work well if the water flows fast enough. If you use a freezer compressor, be careful that your glasswear doesn't implode. I know for a fact that conical flasks do quite easily.
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 08:23 AM
--------------------------------------------------------------------------------
Wonerfull. i really dont care if it burns out after awhile because i can just look for another freezer and take it out again. i have all round bottom flasks and the setup is mabe for vacuum distillations so thres no worry about implosions. heres a pic of the setup:
http://www.unitedglasstech.com/DistillAPPARA24-40-2.jpg (or see attached)
wantsomfet
Frequent Poster
Posts: 239
From: EU
Registered: JAN 2001
posted 07-04-2001 09:02 AM
--------------------------------------------------------------------------------
Nice! Are that TEFLON fittings at the joints?
------------------
for best catfood visit:
kangaroooo.cjb.net
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 12:03 PM
--------------------------------------------------------------------------------
I use a refrigerator compressor i found at a tag sale for $35. An aspirator will work if you use one of those pool pumps to make the water flow, and it can provide a good vacuum and another plus is that you dont need a trap. Those are ground glass fittings wantsomefet, i have the same setup =). And that setup wont implode unless you nick it or force is applied, because ive been vacuum distilling HNO3 about 3 times a week since i got it (1 1/2 months ago) and its still in tip top shape.
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 12:11 PM
--------------------------------------------------------------------------------
Not a bad setup! How much is that costing ya?
I got a load of glasswear very cheap at an army surplus place a few years back. I don't know why it was there, but I got two liebigs, loads of miscellaneous flasks and beakers, connectors, stoppers, etc etc. The whole lot was quite expensive, but a fraction of the new cost.
I got half way towards making one of the condensers (2 feet long) into a CO2 laser, but then gave up. I might finish it some day, because a 200 watt CW laser would be nice to have.
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 02:31 PM
--------------------------------------------------------------------------------
This setup costs $125 US from UGT (unitedglasstech.com). Thats quite low compared to other companies who sell it for around 200 or even more.
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 02:57 PM
--------------------------------------------------------------------------------
I have been talking to some people that have distillation setups similar to mine. One person says that vauum isnt necessar. he claims that when distilled 3 times with conc. H2S04 (tritration) and treated with urea, he can get 99.362% hno3. But i still want to use a vacuum. Does anyone know what kind of tubes i should use with the vacuum?
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-04-2001 03:08 PM
--------------------------------------------------------------------------------
You mean to connect the setup to the pump? You can buy vaccuum tubing from some places that sell glasswear etc, not sure of any specific sources though. A lot depends on what you can attach to the pump and distillation setup. I doubt that a very high vaccuum will be needed, so most tubes will work except soft rubber. Thin glass will work very well if you can attach it.
Although I never used to use a vaccuum to make HNO3 even when I had my pumps. Using a water bath helps to keep the reaction from overheating too much, and the product worked for RDX when decolourised. I'm going to try the Ca(NO3)2 / H2SO4 method, and filter out the CaSO4 and see if that works for RDX. Wish me luck!
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 03:18 PM
--------------------------------------------------------------------------------
Ok, and how do i use urea to perge NOx, NO2, etc? The calcium nitrate method works quite well, ive done it a few times. good luck.
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 05:11 PM
--------------------------------------------------------------------------------
I use 3/8 inch wire reinforced plastic tubing i got from my hardware store. It works really well! A vacuum isnt neccesary, that is correct, but if done correctly you can get concentrated (96%+) HNO3 from just one distillation! To purge HNO3 of urea, just add it in really small amounts until the acid is completely clear, stirring till it dissolves. It wont really polute the acid since i think a concentration higher than 80% of HNO3 will just decompose the urea, although some urea nitrate may form. You usually have to add about 1-2% by weight if your acid is NOx-heavy.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 07-04-2001 06:51 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 07:58 PM
--------------------------------------------------------------------------------
This is really interesting...especially the calcium nitrate + sulfuric method. Can anyone elaborate a bit more on that? Precise procedure? already have a good idea but not completely clear...
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-04-2001 08:09 PM
--------------------------------------------------------------------------------
Its just like kno3 + h2so4 except you use calcium nitrate and it works better than kno3. There is no violent reaction that takes place either.
------------------
How much power will you lose if you do not know what they already know?
Explosives Archive
ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-05-2001 03:39 AM
--------------------------------------------------------------------------------
I can get a very large compressor for large store freezers most likely now. If it's too powerful ill put a dimmer switch to turn the power down. Does anyone have any idea about what to use for traps? im thinking a water trap, then a solid trap with some sodium bicarb and some sort of very hygroscopic material to absorb some of the water. Unles someone else has a more simple plan
------------------
How much power will you lose if you do not know what they already know?
Explosives Archive
[This message has been edited by ALENGOSVIG1 (edited July 05, 2001).]
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-05-2001 07:32 AM
--------------------------------------------------------------------------------
If you can get hold of it, then surround a flask (the trap) with a slurry of dry ice and acetone. This will condense and freeze just about anything, and stop it from getting into the pump.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 07-05-2001 09:21 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Gab
New Member
Posts: 16
From: Québec, Canada
Registered: MAR 2001
posted 07-05-2001 10:26 AM
--------------------------------------------------------------------------------
I have found this picture. It looks like a rather cheap vacuum.
http://www.geocities.com/CapeCanaveral/Lab/4256/2.jpg
[This message has been edited by Gab (edited July 05, 2001).]
SawedOff8gaugeman
Frequent Poster
Posts: 56
From: Finland
Registered: JUN 2001
posted 07-06-2001 04:01 PM
--------------------------------------------------------------------------------
quote:
--------------------------------------------------------------------------------
Originally posted by Mr Cool:
I got half way towards making one of the condensers (2 feet long) into a CO2 laser, but then gave up. I might finish it some day, because a 200 watt CW laser would be nice to have.
--------------------------------------------------------------------------------
Sounds cool!
(This is off-topic ) I would like to know "how to", can you possibly point me to some site or something ??
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 07-06-2001 04:08 PM
--------------------------------------------------------------------------------
I'll e-mail you some stuff on CO2 and other high-power lasers (nitrogen and dye are easy to make.) If anyone else would like some info just ask here.
I made a flashlamp pumped dye laser, and first I used cheap first-surface mirrors. The Al coating on them was almost totally vapourised on the first shot! So I had to pay for better ones. Also the flash lamps exploded every 50 shots or so, because I was putting way too much energy into them. So it all became rather expensive. I'll have to find a way to make my own high-power flash lamps, and start using it again because they're quite fun if you like that sort of thing.