Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2
Author: Subject: Making Nitrous Oxide
thefips
Harmless
*




Posts: 33
Registered: 6-3-2004
Location: Germany
Member Is Offline

Mood: self destructive ;)

[*] posted on 22-8-2004 at 08:56


Yes,my english is not really good... I meant nitric acid,HNO3.
One result from the synthesis of N2O from NH4NO3 is NO2,which is very toxic and it would be difficult to eliminate it from the N2O,because traces will be present.
But in the new synthesis it says,that the N2O is 99,9% pure.
NH4NO3 can explode from strong heating.
View user's profile View All Posts By User
trinitrotoluene
Hazard to Others
***




Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline

Mood: paranoid

[*] posted on 22-8-2004 at 19:10


The problems with whippets are, they're still fairly expensive. One whippet yields enough N2O gas to fill one balloon, that "hit" only produces a 15-30 second effect, then you'll have to use another whippet. So far a box of 24 whippets cost $14.99 so the cost is still very expensive.

It may be cheaper to produce your own nitrous oxide, and with proper purification method, it may be more pure than commercial nitrous from whippets.




TNT
View user's profile View All Posts By User This user has MSN Messenger
thefips
Harmless
*




Posts: 33
Registered: 6-3-2004
Location: Germany
Member Is Offline

Mood: self destructive ;)

[*] posted on 6-9-2004 at 08:54


The reaction works,I tested it the last 2 days.300g sulfuric acid (96%) and 60g urea were mixed in a 500ml round bottomed flask with magnetic stirring.When the urea dissolves the mixture is heated to the reaction temperature.Then 100g of 63% nitric acid are dropped in slowly(!!) with magnetic stirring.The mixture begins to bubble and the gas was washed with NaOH(aq) and collected under water in a big plastic bottle which stood in a bucket of water + Ca(OH)2.The gas was pumped out at the top of the bottle by a compressor of an old fridge and it was pumped again into the bottle,through the Ca(OH)2(aq) but in a lot of small bubbles.A lot of the CO2 was washed out.I tested the Gas and no NO2 was detected,but there was a lot of CO2 in it.

Has someone an idea to wash out the whole CO2?In the gas there are the same amounts of CO2 and N2O and it is to hard to inhale and I think the CO2 is not good for the health...
View user's profile View All Posts By User
Theoretic
International Hazard
*****




Posts: 770
Registered: 17-6-2003
Location: London, the Land of Sun, Summer and Snow
Member Is Offline

Mood: eating the souls of dust mites

[*] posted on 12-9-2004 at 12:29


You could use sulfamic acid instead of urea. You'd then would have to only lightly heat it, and you wouldn't need sulfuric acid



View user's profile View All Posts By User
thefips
Harmless
*




Posts: 33
Registered: 6-3-2004
Location: Germany
Member Is Offline

Mood: self destructive ;)

[*] posted on 12-9-2004 at 19:23


I have stopped all my experiments on the synthesis of N2O.It is a waste of time and it is too difficult to get really pure stuff.And the costs are at the moment higher than a package of N2O capsules which can be bought in the supermarket.
It is better to spend the time on more important syntheses and perhaps other substances would be more fun... :)
View user's profile View All Posts By User
sarcosuchus
Harmless
*




Posts: 25
Registered: 16-9-2004
Location: in server hell
Member Is Offline

Mood: sleepy

[*] posted on 17-9-2004 at 14:26


and thers one way to make NOx that is possible if you have the eq. you will need a plasma cutter,a air compressor, a 5 gal glass water bottle, some copper tubing and misc fittings, 1-2 tig rods and some heavy guage electrical cable,a small water pump(3-5 gpm) a ph tester of some kind and a little creativity. the basic idea is to create a stable arc from the plasma cutter useing the tig rods as the ground while trying not to burn through them too fast.the water pump is to cool the plumbing so as not to have a meltdown durning the operation of the contraption the heavy cable is to complete the circuit so current will flow,copper tubing is used for carring the high temp gas to the water bottle to react with the h2o forming a more storable product:P thers only a couple of thing to remeber 1.its going to be freeking hot 2.lots o current will be in use so if theres a fire DO NOT SPRAY WATER ON ANYTHING:o and make sure thers lots of ventliation in the area you try this.the only tricky thing is postioning the tig rods in a nozzel holding pipe fitting of some kind so the arc is hot but not to hot. just something to think about



famous last words\"hold my beer and watch this\"
View user's profile View All Posts By User
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 17-9-2004 at 14:45


This thread is on the topic of the preparation of N2O not other nitrogen oxides.
View user's profile View All Posts By User
sarcosuchus
Harmless
*




Posts: 25
Registered: 16-9-2004
Location: in server hell
Member Is Offline

Mood: sleepy

[*] posted on 18-9-2004 at 19:47


my line of thinking was somthing like this
Nox+h20=hno3
hn03+aqu.nh3=nh4no3
nh4no3+heat=n2o
more or less what iwas thinking anyway i have a bad tendency to retrosnyth from somthing basic upwards. starting with somthing i know i can make easy.i am allways trying to do somthing in a hurry so as not to see the blue screen of death




famous last words\"hold my beer and watch this\"
View user's profile View All Posts By User
garage chemist
chemical wizard
*****




Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline

Mood: No Mood

[*] posted on 16-1-2005 at 14:23


At the moment, I'm also working on an efficient and economic method for making N2O.

I tried the method from the microscale gas chemistry page and found that it is way too slow. It takes about half an hour to convert half of the AN to N2O.
The produced gas also had a visible brown tint, so this doesn't produce NO2- free N2O either.

The method with urea + HNO3 + H2SO4 is too expensive, the same goes for the hydroxylamine + nitrite reaction.

I have settled on the method of heating pure AN as the production method. The gas evolution is rather fast, depending on the strength of the heating.
The process is carried out in a ground- glass vacuum distillation setup, where the crude N2O comes out of the vacuum adapter.
The produced water vapor condenses in the liebig and is collected in the receiving flask.

I tried this process and it works great, however, the AN must be pure.
The stuff extracted from Kalkamonsalpeter (fertilizer consisting of AN and chalk) cannot be used!
It produces a very nasty impurity which is extremely irritating to the lungs, even in very small concentrations. It is not affected in the slightest even by THOROUGH washing with NaOH. I've got no idea what this could be!
Buy some pure AN, otherwise you will have this nasty stuff in your N2O.

Since 22- 24 liters of N2O are produced from 80g of AN (AN costs only 2,50€ per kg for me), this method is very economic in terms of used chemicals.

However, the problem is not the generation of the N2O, but rather its purification.

The gas contains appreciable quantities of NO2 and NO which must be completely removed.

By bubbling the gas through NaOH soln, the NO2 can be removed. Several washing flasks have to be used in series to remove all of it.

However, NO is not removed this way!
NO doesn't react with bases.
Mixing the N2O with a little air doesn't oxidise all of the NO fast enough because of the great dilution.

I have read that oxidisers like permanganate, dichromate and hypochlorite can oxidise it to NO2.
Permanganate oxidises it quantitatively and this is used as a method of analyzing NO in gas mixes.

So I should probably use a washing boottle with NaOH first, then one with permanganate and then several with NaOH.

How can I find out if the gas still contains NO?
Maybe by smelling it?
I even smell NO2 in car exhausts on the street in the morning when going to school, so I should theoretically be able to detect it.

About storing it:
N2O is surprisingly soluble in water, 1l water will dissolve 1,5l of N2O at 0°C.
When a saturated solution of N2O in water is cooled to its freezing point, crystals with the formula N2O*6H2O crystallize out. They are stable below 0°C and decompose to water and the gas on warming.
This method will of course remove ALL of the NO2, since NO2 reacts with the water rapidly once dissolved.
And NO is quite insoluble in water, 1l dissolves only 70ml.
If the water contains some sodium hypochlorite (maybe hydrogen peroxide works, too?) the NO would be oxidised to nitric acid and on warming the N2O-hydrate crystals, we would get very pure N2O.

I will investigate this in the next few weeks.
I never worked with gas hydrates before, so this will be interesting.
View user's profile View All Posts By User
garage chemist
chemical wizard
*****




Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline

Mood: No Mood

[*] posted on 19-1-2005 at 14:14


I just got some pure AN and started experimenting.
I heated 20g in the described apparatus, it formed a crystal clear melt and decomposed steadily without getting violent. The gas was bubbled through NaOH in a selfmade washing
bottle and smelled totally clean and sweetish, not the slightest hint of NO2.
I filled it into a plastic freezer bag tied to a glass pipe, and when the bag was full, the pipe to the bag was disconnected from the washing bottle.

I smelled the gas, and, sure enough, it strongly smelled of NO2. :mad:

The NO in the crude N2O had reacted with residual air in the plastic bag.

I really need to find a method of absorbing NO!
View user's profile View All Posts By User
miseryland
Harmless
*




Posts: 2
Registered: 28-12-2004
Member Is Offline

Mood: mildly radioact

[*] posted on 19-1-2005 at 15:06
N2O is highly flammable


basic rule, most stuff burns once it reaches a temperature or other condition,
for flurine mere contact with oxygen (not good) for nitrous oxide relatively high temperatures, dont believe me, throw a nos cylinder for nos crackers into a bonfire, oh yes stand behind somethin solid ie a brick wall, schrapnel is not kind to human flesh, and maybe a fire extinguisher just in case
View user's profile View All Posts By User This user has MSN Messenger
Theoretic
International Hazard
*****




Posts: 770
Registered: 17-6-2003
Location: London, the Land of Sun, Summer and Snow
Member Is Offline

Mood: eating the souls of dust mites

[*] posted on 20-1-2005 at 14:28


"N2O is highly flammable

basic rule, most stuff burns once it reaches a temperature or other condition,"

Basic rule, stuff burns if there's an oxidizer to react with. N2O itself is an oxidizer, so it can't burn.

"for flurine mere contact with oxygen (not good)"

When fluorine gets into mere contact with oxygen, nothing happens. They don't react just like that, and for good reason: all of their compounds are endothermic.

"for nitrous oxide relatively high temperatures, dont believe me, throw a nos cylinder for nos crackers into a bonfire, oh yes stand behind somethin solid ie a brick wall, schrapnel is not kind to human flesh, and maybe a fire extinguisher just in case"

Any gas, when confined in a small container and heated, will blow the container and make shrapnel. N2O can additionally exothermically decompose (sometimes explosively, but it's not BURNING!) into N2 and O2, above 500 C I think.




View user's profile View All Posts By User
Polverone
Now celebrating 18 years of madness
*********




Posts: 3164
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline

Mood: Waiting for spring

[*] posted on 27-1-2005 at 20:55
removing NO


The soon-to-be-released DLI book <i>Industrial Nitrogen Compounds and Explosives</i> indicates that NO can be removed from NH4NO3 decomposition products by passing the gas formed through a solution of ferrous sulfate.



PGP Key and corresponding e-mail address
View user's profile Visit user's homepage View All Posts By User
garage chemist
chemical wizard
*****




Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline

Mood: No Mood

[*] posted on 28-1-2005 at 03:25


A-ha! Thanks for the info! I'll try that out soon.

I once saw something similar in a video, where colourless NO (diluted with argon) was bubbled through some iron- salt solution and it formed an intensely blue "pentaaqua-nitrosyleisen" complex.
I wondered if this could be used to absorb NO.

Ferrous sulfate is FeSO4, right?
Can I make it by dissolving iron nails in dilute H2SO4?

How concentrated does the FeSO4- solution have to be?
Does it have to be acidic, or neutral?
View user's profile View All Posts By User
Polverone
Now celebrating 18 years of madness
*********




Posts: 3164
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline

Mood: Waiting for spring

[*] posted on 28-1-2005 at 11:41


Yes, you can make FeSO4 with nails in diluted H2SO4; keep it at least somewhat protected from air of course. I think the scrubbing solution can be acidic or neutral. In one of the arrangements described, NH4NO3 decomposition gases were bubbled through aqueous FeSO4 solution (specifics unspecified) and later dried/cleaned again by passing through a slurry of FeSO4 in conc. H2SO4. NO2 and CO2 were removed by passing through an aqueous mixture of KOH and Ca(OH)2. I presume that CO2 was a minor impurity.



PGP Key and corresponding e-mail address
View user's profile Visit user's homepage View All Posts By User
Mumbles
National Hazard
****




Posts: 436
Registered: 12-3-2003
Location: US
Member Is Offline

Mood: Procrastinating

[*] posted on 28-1-2005 at 17:18


For making ferrous sulfate it is best to use an excess of iron, otherwise the acid will start oxidising it to ferric. Also do it outside as there is SO2 given off. Not pleasant when you just let it react on it's own in the basement. Crashing out with alcohol may be the way to go if you want to isolate it.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
Mindchemist
Harmless
*




Posts: 18
Registered: 27-3-2011
Member Is Offline

Mood: Hydrophobic

[*] posted on 5-4-2011 at 19:16


You could also try the reaction of sodium nitrite and hydroxylammonium chloride to make nitrous oxide:

http://www.youtube.com/watch?v=TGDNm3ENnf8




Wake up and smell the 2-furfuryl mercaptan.
View user's profile View All Posts By User
atomicfire
Harmless
*




Posts: 37
Registered: 7-2-2011
Member Is Offline

Mood: shaprening my molecular scissors

[*] posted on 6-4-2011 at 07:29


Quote: Originally posted by The_Davster  
Heres a pretty easy DIY method;
http://mattson.creighton.edu/N2O/index.html[/url]


I know that guy! He was in graduate school when I was an undergrad. Small world.




ban DHMO
View user's profile View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 3-6-2013 at 09:22


It might not be the most practical preparation, but Nicolai Lehnert at the University of Michigan discovered a di-iron complex that can catalyze the reaction of nitric oxide with nitrogen gas to nitrous oxide at room temperature

http://cen.acs.org/articles/91/i13/Nixing-Nitric-Oxide.html
View user's profile Visit user's homepage View All Posts By User
 Pages:  1  2

  Go To Top