megalomania
June 18th, 2003, 04:09 PM
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-27-2001 09:22 PM
--------------------------------------------------------------------------------
Before i commence the questions, Yes, i have done multiple searches but there are still questions that have gone unanswered, and i dont like the idea of a painful death . Anyway, i have been planning on producing some nitric acid for awhile, but still have some questions i would like answered before i try.
First - Will a good expensive gas mask protect me from noxious gases and the like? (Im not going to put my head up to the receiving flask or anything crazy, but just in case)
Second - I dont have access to jointed glassware, so i am using pyrex and boronsilicate labglass with rubber stoppers. Will the HNO3 or resulting vapors eat at the rubber stoppers? If so, is there any way to acid-proof them? (Possibly by wrapping them tightly in teflon tape, or painting them with teflon if such a thing exists).
Third - The distillation setup is not completely sealed, i have it so it drips into an ehrlenmeyer flask from about an inch above the flask. Will dripping through the air effect the purity at all?
Also, does anyone have an approximate temperature to heat the NaNO3 H2SO4 solution to? (I was thinking possibly 50 or 55*C or would this be too high and decompose the acid before it forms?) Thanks for your time! -John
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-28-2001 12:17 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
PYRO500
Moderator
Posts: 1465
From: somewhere in florida
Registered: SEP 2000
posted 05-28-2001 01:18 AM
--------------------------------------------------------------------------------
just make sure if you need a gas mask to wear a full moon suit but seriously if you notice alot of acid decomposing make sure you are keeping it cool enough (I think) and for emerginceys make sure your cartrages are rated for NOx gasses
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:02 AM
--------------------------------------------------------------------------------
The procedure will be done outside so i guess i dont need a gasmask at all. Hmm, i dont know what to do with the rubber stoppers though. Any way i can get around that? It would be real expensive to buy new glassware. The rubber is very very dense, so perhaps it wont get eaten very fast?
PYRO500
Moderator
Posts: 1465
From: somewhere in florida
Registered: SEP 2000
posted 05-28-2001 02:36 AM
--------------------------------------------------------------------------------
just replace the stopperes, I beleve you can get teflon ones and there is a way to acid proof corks
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:49 AM
--------------------------------------------------------------------------------
Hmm, dont know where i can get teflon stoppers, but i have many corks laying around. Id be interested in hearing that method =)
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 03:01 AM
--------------------------------------------------------------------------------
Hit reply a bit too soon Anyway, i know where to get Teflon stoppers that dont have any holes for volumetric flasks and such, but the stoppers i need must have different sized holes. One goes around a 6mm or so tube that goes into the boiling flask, and the other goes around a 10mm or so tube that goes into the condensor. Corks with drilled holes would probably work.
Here is a pic:
[This message has been edited by John456 (edited May 28, 2001).]
c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 05-28-2001 03:26 AM
--------------------------------------------------------------------------------
If you can get hold of some *wide* teflon tape of the type used on very large threaded pipe (you may have to go to an industrial supply for this) you can use the tape to cover the acid-exposed portions of the rubber stoppers. If you then push the glass tubing right through the teflon into the stopper holes, a "cuff" of the material will wind up squeezed between the glass and the rubber, forming a good seal at the tubing ports. Depending on the temperature, it's even possible polyethylene film might serve the purpose - some of it will stay impervious (even though it gets softer) in boiling water.
As for acid-proofing corks, most chemistry handbooks provide recipes for acid-proofing substances.
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-28-2001 11:42 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:32 PM
--------------------------------------------------------------------------------
I tried it today with 36mL H2SO4 and 58g NaNO3. I put a wide (2 1/2 cm approx) piece of teflon tape around both of the stoppers with the glass tubes poked through it. It looked like it was going fine till a sort of bubble of acid formed under the teflon tape on the rubber stopper. I stopped after about 10 mins after that happened, and the stopper didnt really look eaten too bad, it just looked sort of bumpy. Guess ill just buy some jointed glassware, itll be worth it in the long run.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-05-2001 05:54 PM
--------------------------------------------------------------------------------
Lately, I've been doing some nitric acid distilling. I've got a whole distillation kit so I guess I'm lucky. Screw Rubber stoppers, I have made my own stoppers out of tape and toilet paper, they last longer than you think and don't pollute your acid. I take twice the amount of sulfuric acid and to it add nitric acid of 70% concentration. I then heat it up until I see droplets collecting. I take my product once distillation has finished, and distill it another time, and again if necessary until you get almost pure nitric acid.
Demolition
Frequent Poster
Posts: 158
From: Australia
Registered: FEB 2001
posted 06-06-2001 04:29 AM
--------------------------------------------------------------------------------
Dhzugasvili:With your distillation do you use a vacuum or not?
Demolition
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-06-2001 01:06 PM
--------------------------------------------------------------------------------
http://www.imsplus.com/ims.html
got some nice gas masks, chemical bio hazard/warfare clothes, and even canon fuse
Gab
New Member
Posts: 14
From: Québec, Canada
Registered: MAR 2001
posted 06-07-2001 12:25 AM
--------------------------------------------------------------------------------
You may want to take a look at this MSDS page : http://www.jtbaker.com/msds/n3662.htm.
Here is some excerpts:
Ventilation System:
A system of local and/or general exhaust is recommended to keep employee exposures below the Airborne Exposure Limits.
Personal Respirators (NIOSH Approved):
If the exposure limit is exceeded, wear a supplied air, full-facepiece respirator, airlined hood, or full-facepiece self-contained breathing apparatus. [...]Canister-type respirators using sorbents are ineffective.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-14-2001 06:49 PM
--------------------------------------------------------------------------------
Demolition: I have done the distillations without vacuum. Tried distilling acid twice and thrice but concentration did not rise to acceptable levels, will use NO2 dissolving method instead. From what I hear these vacuum pumps are fucking expensive. You have some way of improvising one or creating lessened pressure?
If anyone is familiar with Sekur filters please reply. I have just bought the B2P2 filter. Will this protect me against NOx fumes? Or do I need the NOP3 filter?
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-14-2001 09:28 PM
--------------------------------------------------------------------------------
Dhzuga, as long as you have a pawn shop or something near you you can pick up a refrigeration pump for $25-75. That might not be the case in Kenya though. I think you can improvise a vacuum pump out of a pool filter pump and some tubing, but i forget the URL. Also, today i distilled some acid under vacuum (using 320mL H2SO4 and 560g NaNO3) and i got a perfectly clear, non fuming acid product. It worked for RDX so i assume it was pretty pure. I didnt see any NOx at all forming in the apparratus like all the other times. I didnt do anything different, so what could have happened?
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-15-2001 03:41 PM
--------------------------------------------------------------------------------
http://cgi.ebay.com/aw-cgi/eBayISAPI.dll?ViewItem&item=1607608602
It's a pretty good deal for a retort...
has anyone had experience distilling HNO3 just using simple retort?
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-15-2001 03:54 PM
--------------------------------------------------------------------------------
I got another confusion, the vacuum pump act as a blower thorough the aspirator, creating lower pressure as air travel faster, hence, no acid fumes is passed through the pump...
so any pump can be used...
I might be wrong but do this really work?
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-15-2001 05:14 PM
--------------------------------------------------------------------------------
I tried distilling some HNO3 with a retort a long time ago. it didnt work too well, most of the vapors just escaped before they had a chance to condensate. As for the vacuum aspirator blowing, i have no idea what you are saying, sorry.
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 06-15-2001 05:45 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-15-2001 10:13 PM
--------------------------------------------------------------------------------
Nope, the aspirator didnt work too well, but it was on a sink. to cool my retort when i used one i cut a hole in the bottom of a plastic bottle and another hole in the lid, as well as two holes on the side. I put the end of the long stem of the retort into the holes in the back and front and tubing from a pump to circulate cool water in the side holes. Something you can make to use with an aspirator that creates a relatively high vacuum (So ive heard, ive never tried it. Id rather use a store bought pump because this method is probably inconsistent) is here: http://rhodium.lycaeum.org/chemistry/equipment/aspirator.html . Id be careful if you do make it though, one minute your acid mix could be fuming nicely and the next it could boil and a bunch of water and NOx vapor will condense over all at once.
[This message has been edited by John456 (edited June 15, 2001).]
Teck
Frequent Poster
Posts: 146
From:
Registered: JAN 2001
posted 06-16-2001 04:20 AM
--------------------------------------------------------------------------------
John456: how much nitric acid did you use and what was your yeild on RDX?
[This message has been edited by Teck (edited June 16, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-17-2001 12:39 AM
--------------------------------------------------------------------------------
The first method on Mega's page, except i used 400mL nitric acid and 75g hexamine. The yield was only about 7 grams but it detonated.
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-27-2001 09:22 PM
--------------------------------------------------------------------------------
Before i commence the questions, Yes, i have done multiple searches but there are still questions that have gone unanswered, and i dont like the idea of a painful death . Anyway, i have been planning on producing some nitric acid for awhile, but still have some questions i would like answered before i try.
First - Will a good expensive gas mask protect me from noxious gases and the like? (Im not going to put my head up to the receiving flask or anything crazy, but just in case)
Second - I dont have access to jointed glassware, so i am using pyrex and boronsilicate labglass with rubber stoppers. Will the HNO3 or resulting vapors eat at the rubber stoppers? If so, is there any way to acid-proof them? (Possibly by wrapping them tightly in teflon tape, or painting them with teflon if such a thing exists).
Third - The distillation setup is not completely sealed, i have it so it drips into an ehrlenmeyer flask from about an inch above the flask. Will dripping through the air effect the purity at all?
Also, does anyone have an approximate temperature to heat the NaNO3 H2SO4 solution to? (I was thinking possibly 50 or 55*C or would this be too high and decompose the acid before it forms?) Thanks for your time! -John
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-28-2001 12:17 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
PYRO500
Moderator
Posts: 1465
From: somewhere in florida
Registered: SEP 2000
posted 05-28-2001 01:18 AM
--------------------------------------------------------------------------------
just make sure if you need a gas mask to wear a full moon suit but seriously if you notice alot of acid decomposing make sure you are keeping it cool enough (I think) and for emerginceys make sure your cartrages are rated for NOx gasses
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:02 AM
--------------------------------------------------------------------------------
The procedure will be done outside so i guess i dont need a gasmask at all. Hmm, i dont know what to do with the rubber stoppers though. Any way i can get around that? It would be real expensive to buy new glassware. The rubber is very very dense, so perhaps it wont get eaten very fast?
PYRO500
Moderator
Posts: 1465
From: somewhere in florida
Registered: SEP 2000
posted 05-28-2001 02:36 AM
--------------------------------------------------------------------------------
just replace the stopperes, I beleve you can get teflon ones and there is a way to acid proof corks
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:49 AM
--------------------------------------------------------------------------------
Hmm, dont know where i can get teflon stoppers, but i have many corks laying around. Id be interested in hearing that method =)
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 03:01 AM
--------------------------------------------------------------------------------
Hit reply a bit too soon Anyway, i know where to get Teflon stoppers that dont have any holes for volumetric flasks and such, but the stoppers i need must have different sized holes. One goes around a 6mm or so tube that goes into the boiling flask, and the other goes around a 10mm or so tube that goes into the condensor. Corks with drilled holes would probably work.
Here is a pic:
[This message has been edited by John456 (edited May 28, 2001).]
c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 05-28-2001 03:26 AM
--------------------------------------------------------------------------------
If you can get hold of some *wide* teflon tape of the type used on very large threaded pipe (you may have to go to an industrial supply for this) you can use the tape to cover the acid-exposed portions of the rubber stoppers. If you then push the glass tubing right through the teflon into the stopper holes, a "cuff" of the material will wind up squeezed between the glass and the rubber, forming a good seal at the tubing ports. Depending on the temperature, it's even possible polyethylene film might serve the purpose - some of it will stay impervious (even though it gets softer) in boiling water.
As for acid-proofing corks, most chemistry handbooks provide recipes for acid-proofing substances.
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-28-2001 11:42 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 05-28-2001 02:32 PM
--------------------------------------------------------------------------------
I tried it today with 36mL H2SO4 and 58g NaNO3. I put a wide (2 1/2 cm approx) piece of teflon tape around both of the stoppers with the glass tubes poked through it. It looked like it was going fine till a sort of bubble of acid formed under the teflon tape on the rubber stopper. I stopped after about 10 mins after that happened, and the stopper didnt really look eaten too bad, it just looked sort of bumpy. Guess ill just buy some jointed glassware, itll be worth it in the long run.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-05-2001 05:54 PM
--------------------------------------------------------------------------------
Lately, I've been doing some nitric acid distilling. I've got a whole distillation kit so I guess I'm lucky. Screw Rubber stoppers, I have made my own stoppers out of tape and toilet paper, they last longer than you think and don't pollute your acid. I take twice the amount of sulfuric acid and to it add nitric acid of 70% concentration. I then heat it up until I see droplets collecting. I take my product once distillation has finished, and distill it another time, and again if necessary until you get almost pure nitric acid.
Demolition
Frequent Poster
Posts: 158
From: Australia
Registered: FEB 2001
posted 06-06-2001 04:29 AM
--------------------------------------------------------------------------------
Dhzugasvili:With your distillation do you use a vacuum or not?
Demolition
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-06-2001 01:06 PM
--------------------------------------------------------------------------------
http://www.imsplus.com/ims.html
got some nice gas masks, chemical bio hazard/warfare clothes, and even canon fuse
Gab
New Member
Posts: 14
From: Québec, Canada
Registered: MAR 2001
posted 06-07-2001 12:25 AM
--------------------------------------------------------------------------------
You may want to take a look at this MSDS page : http://www.jtbaker.com/msds/n3662.htm.
Here is some excerpts:
Ventilation System:
A system of local and/or general exhaust is recommended to keep employee exposures below the Airborne Exposure Limits.
Personal Respirators (NIOSH Approved):
If the exposure limit is exceeded, wear a supplied air, full-facepiece respirator, airlined hood, or full-facepiece self-contained breathing apparatus. [...]Canister-type respirators using sorbents are ineffective.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-14-2001 06:49 PM
--------------------------------------------------------------------------------
Demolition: I have done the distillations without vacuum. Tried distilling acid twice and thrice but concentration did not rise to acceptable levels, will use NO2 dissolving method instead. From what I hear these vacuum pumps are fucking expensive. You have some way of improvising one or creating lessened pressure?
If anyone is familiar with Sekur filters please reply. I have just bought the B2P2 filter. Will this protect me against NOx fumes? Or do I need the NOP3 filter?
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-14-2001 09:28 PM
--------------------------------------------------------------------------------
Dhzuga, as long as you have a pawn shop or something near you you can pick up a refrigeration pump for $25-75. That might not be the case in Kenya though. I think you can improvise a vacuum pump out of a pool filter pump and some tubing, but i forget the URL. Also, today i distilled some acid under vacuum (using 320mL H2SO4 and 560g NaNO3) and i got a perfectly clear, non fuming acid product. It worked for RDX so i assume it was pretty pure. I didnt see any NOx at all forming in the apparratus like all the other times. I didnt do anything different, so what could have happened?
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-15-2001 03:41 PM
--------------------------------------------------------------------------------
http://cgi.ebay.com/aw-cgi/eBayISAPI.dll?ViewItem&item=1607608602
It's a pretty good deal for a retort...
has anyone had experience distilling HNO3 just using simple retort?
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-15-2001 03:54 PM
--------------------------------------------------------------------------------
I got another confusion, the vacuum pump act as a blower thorough the aspirator, creating lower pressure as air travel faster, hence, no acid fumes is passed through the pump...
so any pump can be used...
I might be wrong but do this really work?
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-15-2001 05:14 PM
--------------------------------------------------------------------------------
I tried distilling some HNO3 with a retort a long time ago. it didnt work too well, most of the vapors just escaped before they had a chance to condensate. As for the vacuum aspirator blowing, i have no idea what you are saying, sorry.
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 06-15-2001 05:45 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-15-2001 10:13 PM
--------------------------------------------------------------------------------
Nope, the aspirator didnt work too well, but it was on a sink. to cool my retort when i used one i cut a hole in the bottom of a plastic bottle and another hole in the lid, as well as two holes on the side. I put the end of the long stem of the retort into the holes in the back and front and tubing from a pump to circulate cool water in the side holes. Something you can make to use with an aspirator that creates a relatively high vacuum (So ive heard, ive never tried it. Id rather use a store bought pump because this method is probably inconsistent) is here: http://rhodium.lycaeum.org/chemistry/equipment/aspirator.html . Id be careful if you do make it though, one minute your acid mix could be fuming nicely and the next it could boil and a bunch of water and NOx vapor will condense over all at once.
[This message has been edited by John456 (edited June 15, 2001).]
Teck
Frequent Poster
Posts: 146
From:
Registered: JAN 2001
posted 06-16-2001 04:20 AM
--------------------------------------------------------------------------------
John456: how much nitric acid did you use and what was your yeild on RDX?
[This message has been edited by Teck (edited June 16, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-17-2001 12:39 AM
--------------------------------------------------------------------------------
The first method on Mega's page, except i used 400mL nitric acid and 75g hexamine. The yield was only about 7 grams but it detonated.