megalomania
June 21st, 2003, 01:37 PM
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-21-2001 04:41 PM
--------------------------------------------------------------------------------
I Was just wondering if there is any way to:
a) improvise a home made vacuum pump
b) MAKE NITRIC ACID OF 95% CONC. OR MORE WITHOUT A VACUUM PUMP OR SIMILAR DEVICE.
I would be *grateful* if any of you that have succeeded in making RED NITRIC acid without a vacuum pump share your knowledge with me, or any of you that have made an improvised pump tell me about it.
I have no problem acquiring most chemicals... but this one has proven to be a bit of a problem...what is red nitric used for in the industry so if I find a place that sells it and they ask me what I want it for I may provide them with explanation.
simply RED
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Posts: 242
From: HELL
Registered: OCT 2000
posted 06-21-2001 06:46 PM
--------------------------------------------------------------------------------
I haven't made clear 95-100 HNO3 in good quantities and it seems difficult to do it in high quantities at home. The process with the 2 bottles and KNO3/ H2SO4 distilling seems good.
Azotna kisilina - towa e mateql koito maika si ebal. hehehehhehe
(what a nasty work is to find conc HNO3)
Can someone translate bulgarian?
mongo blongo
Frequent Poster
Posts: 175
From: I live in a Creosote Bush!
Registered: JUN 2001
posted 06-21-2001 08:27 PM
--------------------------------------------------------------------------------
dude, u want to make RED nitric acid? as far as i know the reason you need a vacuum is because water and nitric oxides get in the acid from a normal atmosfear (the nitric oxides turn the nitric acid the red colour!)
but i do have an idea ( i have never tried it and don't know if it will work)
if you can somehow carry out the experement in an air tight atmosfear and put a bowl of anhydrous copper sulphate (white not blue) in there the water from the surroundings will be absorbed ( turning the copper sulphate blue) and then you will have less water in your nitric acid
you could also use something like sillica gel
instead of copper sulphate!
but i have no ideas to keep the nitric oxides out
Teck
Frequent Poster
Posts: 146
From:
Registered: JAN 2001
posted 06-22-2001 02:23 AM
--------------------------------------------------------------------------------
All pure acids are clear in color, and if your acid is red or whatever other color then it isnt pure and isnt as good as the clear stuff. Anyone correct me if Im wrong.
Mr Cool
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Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-22-2001 01:50 PM
--------------------------------------------------------------------------------
I assume you're not including picric acid etc etc etc etc.
All mineral acids are clear when pure, maybe?
Nitrogen oxides are formed by decomposition of the HNO3 in the still, they don't come from the air.
I've made red, very strong nitric acid with a normal glass retort, no vaccuum. It gelatinised normal cellulose fibres into a sticky yellow blob! It also worked for RDX when urea was added.
frostfire
Frequent Poster
Posts: 267
From:
Registered: SEP 2000
posted 06-22-2001 02:36 PM
--------------------------------------------------------------------------------
wait a minute,
is the glass retort the one with only single glass bulb and glass pipe going down from the top at an angle......do you put anything else
beside HNO3 70% or xNO3 and H2SO4?
How'd the red fuming got produced?
I read from at.engr.exp (catfood site) that even the guy is struggling with a vacuum distillation to get that thing
I've tried also the two joined glass bottle but end up with not even fuming clear acid and a broken (not braking) bottle
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-22-2001 03:54 PM
--------------------------------------------------------------------------------
I beleive this has been discussed before but recently ive been experimenting with converting ammonia to NOx gas by catylyzing with platinum-rhodium pieces i got from old catylitic converters found in cars. The device i have built consists of a flat-bottom 24/40 florence flask thats filled with 30% ammonium hydroxide solution and capped with a thermometer adapter on a hotplate. In the adapter a length of glass tubing is extended and put into a small (3 inch) length of flexible tubing that fits over some steel tubing of 1 inch diameter. The steel tubing goes for a couple of feet so the rubber tubing doesnt get hot and melt. The steel tubing is then connected to a 3-way steel pipe with a 3-inch diameter that is shaped like an upside down T and has a threaded hole on the top and two threaded holes on the sides, and runs through an old gas grill. The tubing is put in one of the threaded holes about 6 inches in, leaving a good sized space for air. The other side has a threaded adapter that screws in to fit 1-inch pipe. A right angled pipe is put into a hole in a 2 1/2 or so diameter rubber stopper that fits into a jar i made, and flexible tubing with lots of holes in it (to lessen the pull of vacuum significantly) goes into another hole in that same stopper that is connected to a vacuum pump. When the ammonium hydroxide solution starts boiling and a good amount of ammonia gas is passing through the pipe pieces of platinum-rhodium in a steel pan are then heated on a gas burner until they are red-hot (it takes a while), and funnelled into the top hole in the steel pipe. The steel pipe (which has been heating on medium heat on the grill) is then capped and the vacuum pump is turned on. The ammonia gas touches the red-hot platinum-rhodium pieces and turns into NOx and a couple other things will be produced and when it is bubbled through the water in the jar nitric acid is formed. The vacuum pulls air from the hole in the pipe so the reaction can continue and to make sure the NOx gets bubbled through the water. Theoretically you can make 100% acid with free NOx (fuming) with this setup! Ive just started experimenting with it and the max conc acid ive been able to make is about 23% (But thats pretty damn good starting off with nothing but ammonium hydroxide), seems like some ammonia is still getting by unreacted. I know this requires a vacuum source but i thought you guys would be interested in it since i saw old threads discussing it but nobody ever said they tried it and i didnt want to start a new thread. Heres a picture i drew in paint to illustrate it (i hope the mods dont get pissed at me for posting a pic).
Edit: fixed the pic link
[This message has been edited by John456 (edited June 22, 2001).]
Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 06-22-2001 08:20 PM
--------------------------------------------------------------------------------
Nothing worng with posting a picture, especially when it's as original as this.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 05:33 AM
--------------------------------------------------------------------------------
Simply Red, that's some pretty good Bulgarian! If you say you made the Hno3 but not in good quantities how did you get it in small quantities in the first place? Mr. Cool, what where your distilling reactants? Kno3 and H2So4 or Nh4No3 and H2so4?
Confuscious once said: "Mierda, puta! Has de creer que estoy enfermo!"
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-23-2001 09:00 AM
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*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
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Posts: 105
From:
Registered: MAR 2001
posted 06-23-2001 10:48 AM
--------------------------------------------------------------------------------
Hmm, regulating the temp might be a problem since i dont think the grill gets that hot. Might have to buy some type of small furnace. As for oxygen entering the vacuum pulls it through the steel pipe with the ammonia gas. What should i use for drying? I have some potassium polyacryate gel i use for dessicating all the time, ill fasten a drying tube out of metal and put it at the end of the steel pipe. For cooling the gas im using NH4NO3 and water, with the exit tube passing through a bucket of it.
[This message has been edited by John456 (edited June 23, 2001).]
Dhzugasvili
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Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 12:41 PM
--------------------------------------------------------------------------------
Drazvitzie All! I realize this is quite a long reply, but it would really be enlightening if you take some of your time read it. John456, do you have access to dilute nitric acid? Because if you do I am sure you are aware that you can get NO2 out of it by adding formol, all you would need to do then is pass the glass tubing into another flask containing water to make nitric acid and also bubble in some O2 to make the yield greater. You would need to put it in a salt ice water bath for better absorption. This method has gotten for me two results: 1) when bubbled with the O2, the acid appeared dark yellow and it fumed NO2. 2) when bubbled with only NO2, without O2, I got a dark green solution of heavily fuming acid.
So that sucks because it doesn't give me the desired product, 95% or more concentration of nitric acid. I have tried distillations without vacuums. I have tried the following: 1) distilling 100ml 70% Nitric with 200ml 98% sulfuric. the product was an orange acid that fumed NO2.
2) distilling that product from the above a second time. the same product was obtained with no apparent raise in the concentration.
3) distilling KNo3 with 98% H2So4. The product was the same, orange acid that fumed NO2.
4) distilling the dark green acid produced from the bubbling NO2 process. INTERESTINGLY ENOUGH, this gave me some REALLY CONCENTRATED RED/GREEN ACID. But then I had to stop procedure because I had to go. I wonder if it would have continued to give me the same product. now this is an interesting product, dark green/RED nitric acid, and it DOES gelatinize cotton. My only problem with this is that it is a little green, I wonder why. Will keep on trying since this has proven to be the most productive process.
I doubt any of the ORange products are 95%+ Nitric Acid. I have not tried to see if they gelatinize cotton though. ANy imput will be appreciated.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 12:45 PM
--------------------------------------------------------------------------------
...I forgot one more thing. I will try to distill sulfuric (98%) with ammonium nitrate. Is this process recommended?
John456
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Posts: 105
From:
Registered: MAR 2001
posted 06-23-2001 01:49 PM
--------------------------------------------------------------------------------
Yes, i have access to dilute HNO3 but distilling H2SO4/NaNO3 makes a better product with better yield too. Ive succeeded in making acid from that procedure so now im interested in making it cheaply and efficiently.
PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 06-23-2001 02:53 PM
--------------------------------------------------------------------------------
I am guessing you acid may be green due to copper in your distillation apparatus, or other impurities though could cause your wierd NA.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-24-2001 12:40 AM
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*
[This message has been edited by 10fingers (edited October 26, 2001).]
Mr Cool
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Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-24-2001 12:13 PM
--------------------------------------------------------------------------------
Yes, I used a plain glass retort. One bulb, one long glass delivery tube. Reactants were c. 100% H2SO4 (heated until it boiled, and used as soon as it had cooled) and dry KNO3. Product was deep orange/red, and strongly fumed brown mist (not just NO2 gas, it was cloudy HNO3 vapour as well).
A gas flame will reach well over 1000*C with enough air. Pure oxygen won't be needed. However, you may have trouble heating an object to this temperature, since as it gets hotter it'll lose heat faster!
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-24-2001 02:06 PM
--------------------------------------------------------------------------------
When i heat the plat-rhod pieces they should get hot enough for the reaction (about 800*C im guessing) and since its an exothermic reaction it should produce its own heat. THe grill is just there to minimize heat loss during the reaction. I modified the apparatus so there are more holes in the tube going to the vacuum to lessen the pull more. It seems there is more NOx coming through the water than before. With 800mL of boiling hydroxide solution (30%) i was able to make 200mL of 40% nitric acid, and i still have some hydroxide left over because i had to turn the vacuum off for danger of overheating. I was able to heat this acid down to 70% and then vacuum distill it with sulfuric acid to obtain conc. 92% or so acid! All from ammonium hydroxide . The problems now are that eventually the reaction would lose enough heat to stop converting the gas, which would stop the reaction all together and ammonia would come in and neutralize my acid. Also, the vacuum pump seems to get quite hot quicker than normal so im worried it could overheat.
Edit: Oh yeah, the steel tube now goes through an elevated bucket with a hole cut in the bottom that has a cold-pak style mixture of NH4NO3 and water.
[This message has been edited by John456 (edited June 24, 2001).]
frostfire
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Posts: 267
From:
Registered: SEP 2000
posted 06-24-2001 06:07 PM
--------------------------------------------------------------------------------
thx Mr. Cool, now I'm ready to buy one with a expereience reference.
Dhzugasvili,
that's a very interesting documentation but that green color is very weird....i've never seen anything like it in nitric acid distillation
[This message has been edited by frostfire (edited June 25, 2001).]
Bitter
Frequent Poster
Posts: 292
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 06-26-2001 03:06 PM
--------------------------------------------------------------------------------
There isn't any stainless steel in your apparatus is there ? Nickel salts are usually green in colour.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-03-2001 06:26 PM
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According to the info I have read so far, the best, and hopefully SURE SHIT way to make NA of high concentration would be to distill NaNo3, Nh4No3, or kno3, HNO3 with sulfuric acid and with a vacuum. HOW CAN I IMPROVISE A VACUUM? I thought of a very long bike pump but not too sure about that...
to check the concentration of the acid, what do I need to do? I have tried this distillation without a vacuum and i do not get a red color, but a light orange color (like oranges!) could this be highly concentrated acid? what is the viscosity of highly 95%+ concentrated NA? In comparison to water, 98% sulfuric acid, and 70% NA? NH4no3 + H2so4 yield of acid is higher in concentration than kno3 sulfuric A. yield?
10fingers
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Posts: 415
From: USA
Registered: SEP 2000
posted 07-03-2001 07:14 PM
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*
[This message has been edited by 10fingers (edited October 26, 2001).]
PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-03-2001 08:51 PM
--------------------------------------------------------------------------------
I designed a vaccume still, but I don't know if any of the components would react with your product, anyways, a picture of it is here. "http://www.geocities.com/pyro2000us/hno3.jpg"
simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 07-04-2001 06:13 AM
--------------------------------------------------------------------------------
I've made conc. nitric acid with KNO3-H2SO4 distiling and Pb(NO3)2 H2SO4 heating and decanting. It is concentrated and works for nitrating alcohols but not for RDX .
Sorry for the late reply. I had work with the urea fertilizer .
Dzugasvili otde znae6 bylgarskiq. Pi6i edno pismo ako iska6.(Where do you know the bulgarian from, Dzugasvili) .
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 07:42 PM
--------------------------------------------------------------------------------
Impressive...I'm a Rusky, but not living in Mother Rossia, living in Kenya, but anyways, know a bit of Bulgarian too. Ah! SLAvIA...Vissarionovic was aLmIghTy leader...
KatYa Gordeeva is my name...NIET!
Dhzugasvili
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Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 08:14 PM
--------------------------------------------------------------------------------
Thank you for the link, Pyro500.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-05-2001 06:15 PM
--------------------------------------------------------------------------------
IM SUCH A STUPID FUCK!!!!!!! Guess what people, fuck the vacuum, I did the stupidest thing, and all this time I have been trying to produce 95% Nitric Acid when I had it all along!!!! I hadn't tried to check the density and I checked the density of my ORANGE nitric acid that was distilled from sulfuric twice, and guess what, 1.53 density with percentage error accounted for. 30ml of nitric weighed exactly 46g, so that divided by 30 is the density. NEXT with this very same acid I tried pouring a tiny amount on some cotton...it gelatinized the fuck out of it!! Yellow sticky blob just like your product Mr. Cool. The acid fumes white and red fumes rather heavily. hooray! on to synthesis...
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-21-2001 04:41 PM
--------------------------------------------------------------------------------
I Was just wondering if there is any way to:
a) improvise a home made vacuum pump
b) MAKE NITRIC ACID OF 95% CONC. OR MORE WITHOUT A VACUUM PUMP OR SIMILAR DEVICE.
I would be *grateful* if any of you that have succeeded in making RED NITRIC acid without a vacuum pump share your knowledge with me, or any of you that have made an improvised pump tell me about it.
I have no problem acquiring most chemicals... but this one has proven to be a bit of a problem...what is red nitric used for in the industry so if I find a place that sells it and they ask me what I want it for I may provide them with explanation.
simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 06-21-2001 06:46 PM
--------------------------------------------------------------------------------
I haven't made clear 95-100 HNO3 in good quantities and it seems difficult to do it in high quantities at home. The process with the 2 bottles and KNO3/ H2SO4 distilling seems good.
Azotna kisilina - towa e mateql koito maika si ebal. hehehehhehe
(what a nasty work is to find conc HNO3)
Can someone translate bulgarian?
mongo blongo
Frequent Poster
Posts: 175
From: I live in a Creosote Bush!
Registered: JUN 2001
posted 06-21-2001 08:27 PM
--------------------------------------------------------------------------------
dude, u want to make RED nitric acid? as far as i know the reason you need a vacuum is because water and nitric oxides get in the acid from a normal atmosfear (the nitric oxides turn the nitric acid the red colour!)
but i do have an idea ( i have never tried it and don't know if it will work)
if you can somehow carry out the experement in an air tight atmosfear and put a bowl of anhydrous copper sulphate (white not blue) in there the water from the surroundings will be absorbed ( turning the copper sulphate blue) and then you will have less water in your nitric acid
you could also use something like sillica gel
instead of copper sulphate!
but i have no ideas to keep the nitric oxides out
Teck
Frequent Poster
Posts: 146
From:
Registered: JAN 2001
posted 06-22-2001 02:23 AM
--------------------------------------------------------------------------------
All pure acids are clear in color, and if your acid is red or whatever other color then it isnt pure and isnt as good as the clear stuff. Anyone correct me if Im wrong.
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-22-2001 01:50 PM
--------------------------------------------------------------------------------
I assume you're not including picric acid etc etc etc etc.
All mineral acids are clear when pure, maybe?
Nitrogen oxides are formed by decomposition of the HNO3 in the still, they don't come from the air.
I've made red, very strong nitric acid with a normal glass retort, no vaccuum. It gelatinised normal cellulose fibres into a sticky yellow blob! It also worked for RDX when urea was added.
frostfire
Frequent Poster
Posts: 267
From:
Registered: SEP 2000
posted 06-22-2001 02:36 PM
--------------------------------------------------------------------------------
wait a minute,
is the glass retort the one with only single glass bulb and glass pipe going down from the top at an angle......do you put anything else
beside HNO3 70% or xNO3 and H2SO4?
How'd the red fuming got produced?
I read from at.engr.exp (catfood site) that even the guy is struggling with a vacuum distillation to get that thing
I've tried also the two joined glass bottle but end up with not even fuming clear acid and a broken (not braking) bottle
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-22-2001 03:54 PM
--------------------------------------------------------------------------------
I beleive this has been discussed before but recently ive been experimenting with converting ammonia to NOx gas by catylyzing with platinum-rhodium pieces i got from old catylitic converters found in cars. The device i have built consists of a flat-bottom 24/40 florence flask thats filled with 30% ammonium hydroxide solution and capped with a thermometer adapter on a hotplate. In the adapter a length of glass tubing is extended and put into a small (3 inch) length of flexible tubing that fits over some steel tubing of 1 inch diameter. The steel tubing goes for a couple of feet so the rubber tubing doesnt get hot and melt. The steel tubing is then connected to a 3-way steel pipe with a 3-inch diameter that is shaped like an upside down T and has a threaded hole on the top and two threaded holes on the sides, and runs through an old gas grill. The tubing is put in one of the threaded holes about 6 inches in, leaving a good sized space for air. The other side has a threaded adapter that screws in to fit 1-inch pipe. A right angled pipe is put into a hole in a 2 1/2 or so diameter rubber stopper that fits into a jar i made, and flexible tubing with lots of holes in it (to lessen the pull of vacuum significantly) goes into another hole in that same stopper that is connected to a vacuum pump. When the ammonium hydroxide solution starts boiling and a good amount of ammonia gas is passing through the pipe pieces of platinum-rhodium in a steel pan are then heated on a gas burner until they are red-hot (it takes a while), and funnelled into the top hole in the steel pipe. The steel pipe (which has been heating on medium heat on the grill) is then capped and the vacuum pump is turned on. The ammonia gas touches the red-hot platinum-rhodium pieces and turns into NOx and a couple other things will be produced and when it is bubbled through the water in the jar nitric acid is formed. The vacuum pulls air from the hole in the pipe so the reaction can continue and to make sure the NOx gets bubbled through the water. Theoretically you can make 100% acid with free NOx (fuming) with this setup! Ive just started experimenting with it and the max conc acid ive been able to make is about 23% (But thats pretty damn good starting off with nothing but ammonium hydroxide), seems like some ammonia is still getting by unreacted. I know this requires a vacuum source but i thought you guys would be interested in it since i saw old threads discussing it but nobody ever said they tried it and i didnt want to start a new thread. Heres a picture i drew in paint to illustrate it (i hope the mods dont get pissed at me for posting a pic).
Edit: fixed the pic link
[This message has been edited by John456 (edited June 22, 2001).]
Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 06-22-2001 08:20 PM
--------------------------------------------------------------------------------
Nothing worng with posting a picture, especially when it's as original as this.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 05:33 AM
--------------------------------------------------------------------------------
Simply Red, that's some pretty good Bulgarian! If you say you made the Hno3 but not in good quantities how did you get it in small quantities in the first place? Mr. Cool, what where your distilling reactants? Kno3 and H2So4 or Nh4No3 and H2so4?
Confuscious once said: "Mierda, puta! Has de creer que estoy enfermo!"
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-23-2001 09:00 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-23-2001 10:48 AM
--------------------------------------------------------------------------------
Hmm, regulating the temp might be a problem since i dont think the grill gets that hot. Might have to buy some type of small furnace. As for oxygen entering the vacuum pulls it through the steel pipe with the ammonia gas. What should i use for drying? I have some potassium polyacryate gel i use for dessicating all the time, ill fasten a drying tube out of metal and put it at the end of the steel pipe. For cooling the gas im using NH4NO3 and water, with the exit tube passing through a bucket of it.
[This message has been edited by John456 (edited June 23, 2001).]
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 12:41 PM
--------------------------------------------------------------------------------
Drazvitzie All! I realize this is quite a long reply, but it would really be enlightening if you take some of your time read it. John456, do you have access to dilute nitric acid? Because if you do I am sure you are aware that you can get NO2 out of it by adding formol, all you would need to do then is pass the glass tubing into another flask containing water to make nitric acid and also bubble in some O2 to make the yield greater. You would need to put it in a salt ice water bath for better absorption. This method has gotten for me two results: 1) when bubbled with the O2, the acid appeared dark yellow and it fumed NO2. 2) when bubbled with only NO2, without O2, I got a dark green solution of heavily fuming acid.
So that sucks because it doesn't give me the desired product, 95% or more concentration of nitric acid. I have tried distillations without vacuums. I have tried the following: 1) distilling 100ml 70% Nitric with 200ml 98% sulfuric. the product was an orange acid that fumed NO2.
2) distilling that product from the above a second time. the same product was obtained with no apparent raise in the concentration.
3) distilling KNo3 with 98% H2So4. The product was the same, orange acid that fumed NO2.
4) distilling the dark green acid produced from the bubbling NO2 process. INTERESTINGLY ENOUGH, this gave me some REALLY CONCENTRATED RED/GREEN ACID. But then I had to stop procedure because I had to go. I wonder if it would have continued to give me the same product. now this is an interesting product, dark green/RED nitric acid, and it DOES gelatinize cotton. My only problem with this is that it is a little green, I wonder why. Will keep on trying since this has proven to be the most productive process.
I doubt any of the ORange products are 95%+ Nitric Acid. I have not tried to see if they gelatinize cotton though. ANy imput will be appreciated.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-23-2001 12:45 PM
--------------------------------------------------------------------------------
...I forgot one more thing. I will try to distill sulfuric (98%) with ammonium nitrate. Is this process recommended?
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-23-2001 01:49 PM
--------------------------------------------------------------------------------
Yes, i have access to dilute HNO3 but distilling H2SO4/NaNO3 makes a better product with better yield too. Ive succeeded in making acid from that procedure so now im interested in making it cheaply and efficiently.
PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 06-23-2001 02:53 PM
--------------------------------------------------------------------------------
I am guessing you acid may be green due to copper in your distillation apparatus, or other impurities though could cause your wierd NA.
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-24-2001 12:40 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-24-2001 12:13 PM
--------------------------------------------------------------------------------
Yes, I used a plain glass retort. One bulb, one long glass delivery tube. Reactants were c. 100% H2SO4 (heated until it boiled, and used as soon as it had cooled) and dry KNO3. Product was deep orange/red, and strongly fumed brown mist (not just NO2 gas, it was cloudy HNO3 vapour as well).
A gas flame will reach well over 1000*C with enough air. Pure oxygen won't be needed. However, you may have trouble heating an object to this temperature, since as it gets hotter it'll lose heat faster!
John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 06-24-2001 02:06 PM
--------------------------------------------------------------------------------
When i heat the plat-rhod pieces they should get hot enough for the reaction (about 800*C im guessing) and since its an exothermic reaction it should produce its own heat. THe grill is just there to minimize heat loss during the reaction. I modified the apparatus so there are more holes in the tube going to the vacuum to lessen the pull more. It seems there is more NOx coming through the water than before. With 800mL of boiling hydroxide solution (30%) i was able to make 200mL of 40% nitric acid, and i still have some hydroxide left over because i had to turn the vacuum off for danger of overheating. I was able to heat this acid down to 70% and then vacuum distill it with sulfuric acid to obtain conc. 92% or so acid! All from ammonium hydroxide . The problems now are that eventually the reaction would lose enough heat to stop converting the gas, which would stop the reaction all together and ammonia would come in and neutralize my acid. Also, the vacuum pump seems to get quite hot quicker than normal so im worried it could overheat.
Edit: Oh yeah, the steel tube now goes through an elevated bucket with a hole cut in the bottom that has a cold-pak style mixture of NH4NO3 and water.
[This message has been edited by John456 (edited June 24, 2001).]
frostfire
Frequent Poster
Posts: 267
From:
Registered: SEP 2000
posted 06-24-2001 06:07 PM
--------------------------------------------------------------------------------
thx Mr. Cool, now I'm ready to buy one with a expereience reference.
Dhzugasvili,
that's a very interesting documentation but that green color is very weird....i've never seen anything like it in nitric acid distillation
[This message has been edited by frostfire (edited June 25, 2001).]
Bitter
Frequent Poster
Posts: 292
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 06-26-2001 03:06 PM
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There isn't any stainless steel in your apparatus is there ? Nickel salts are usually green in colour.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-03-2001 06:26 PM
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According to the info I have read so far, the best, and hopefully SURE SHIT way to make NA of high concentration would be to distill NaNo3, Nh4No3, or kno3, HNO3 with sulfuric acid and with a vacuum. HOW CAN I IMPROVISE A VACUUM? I thought of a very long bike pump but not too sure about that...
to check the concentration of the acid, what do I need to do? I have tried this distillation without a vacuum and i do not get a red color, but a light orange color (like oranges!) could this be highly concentrated acid? what is the viscosity of highly 95%+ concentrated NA? In comparison to water, 98% sulfuric acid, and 70% NA? NH4no3 + H2so4 yield of acid is higher in concentration than kno3 sulfuric A. yield?
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 07-03-2001 07:14 PM
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[This message has been edited by 10fingers (edited October 26, 2001).]
PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-03-2001 08:51 PM
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I designed a vaccume still, but I don't know if any of the components would react with your product, anyways, a picture of it is here. "http://www.geocities.com/pyro2000us/hno3.jpg"
simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 07-04-2001 06:13 AM
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I've made conc. nitric acid with KNO3-H2SO4 distiling and Pb(NO3)2 H2SO4 heating and decanting. It is concentrated and works for nitrating alcohols but not for RDX .
Sorry for the late reply. I had work with the urea fertilizer .
Dzugasvili otde znae6 bylgarskiq. Pi6i edno pismo ako iska6.(Where do you know the bulgarian from, Dzugasvili) .
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 07:42 PM
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Impressive...I'm a Rusky, but not living in Mother Rossia, living in Kenya, but anyways, know a bit of Bulgarian too. Ah! SLAvIA...Vissarionovic was aLmIghTy leader...
KatYa Gordeeva is my name...NIET!
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-04-2001 08:14 PM
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Thank you for the link, Pyro500.
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-05-2001 06:15 PM
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IM SUCH A STUPID FUCK!!!!!!! Guess what people, fuck the vacuum, I did the stupidest thing, and all this time I have been trying to produce 95% Nitric Acid when I had it all along!!!! I hadn't tried to check the density and I checked the density of my ORANGE nitric acid that was distilled from sulfuric twice, and guess what, 1.53 density with percentage error accounted for. 30ml of nitric weighed exactly 46g, so that divided by 30 is the density. NEXT with this very same acid I tried pouring a tiny amount on some cotton...it gelatinized the fuck out of it!! Yellow sticky blob just like your product Mr. Cool. The acid fumes white and red fumes rather heavily. hooray! on to synthesis...