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thefips
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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.
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trinitrotoluene
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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
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thefips
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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...
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Theoretic
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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
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thefips
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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... 
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sarcosuchus
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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 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 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\"
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The_Davster
A pnictogen
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This thread is on the topic of the preparation of N2O not other nitrogen oxides.
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sarcosuchus
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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\"
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garage chemist
chemical wizard
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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.
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garage chemist
chemical wizard
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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. 
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!
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miseryland
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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
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Theoretic
National Hazard
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"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.
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Polverone
Now celebrating 21 years of madness
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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
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garage chemist
chemical wizard
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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?
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Polverone
Now celebrating 21 years of madness
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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
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Mumbles
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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.
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Mindchemist
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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.
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atomicfire
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I know that guy! He was in graduate school when I was an undergrad. Small world.
ban DHMO
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AndersHoveland
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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
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