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DoctorZET
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If you add to a nitrate salt (fine powdered) some SO3 at a very low temperature and high pressure (not to high, 2-4 atm is enough), you could get in a
long period of time (very loooong period) some traces of N2O5... but is not a good method if you want make some signifiant quantities of N2O5...
My big problem is that I can not find a better method of making N2O5 (without of using P2O5 because I can make this chemical very hard - look in the
phosphorus section ~LINK: https://www.sciencemadness.org/whisper/viewthread.php?tid=65... ~ from where I got white phosphorus, I'm sure you will find that ammusant)...an
other instead of bubbling a rich ozone containing mixture (approx: 20-30% O3 70-80% O2) in a long flask filled with N2O4 (liquid)...
And my second problem is that I not have an actual source for making nitrates or N-compounds... I using the freaking N2 from air and O2 from air and
water...and for the amino-compounds I use NH4HCO3, yes that's my source of ammonia...baking powder 
An other problem...wich I can not solve yet...is that I need N2O5 for organic reactions (to avoid using H2SO4)...and I need to be as pure as possible,
to avoid side-reactions with NO2 or other impurities...and because of it's high-purity, I can dissolve white crystals of N2O5 in water, until I have
HNO3 100%, and then I can dissolve N2O5 in HNO3 until I have a saturated solution...so I can get a form of pure white fuming nitric acid wich is hard
to get through other methods...but I also need a better method, because I spend 24H just to make a few milliliters (35-40 ml) of white fuming
HNO3...that's freaking annoying...
Soooo...if is somebody here who can tell me an other-ways-to-whiteN2O5, I'll be very happy 
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Zyklon-A
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N2O5 can be made from N2O4 and ozone.
Here's some more methods:http://nitrogen.atomistry.com/nitrogen_pentoxide.html
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S.C. Wack
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The thread bfesser should have locked. Do you really think it was intended to be a place to ask all the methods for preparing N2O5 from air and I
don't know, a burned out match, no doubt for RDX (from ammonium bicarbonate of course)? And in response post the same links over and over? I'm
obviously the only one who despises new members (who post) more and more every year, but still...
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DoctorZET
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Well, I'm sorry for the stains leaved on the wall of this forum ... but, over all, this is a place to ask about nitric acid, its compounds and how to
make those two ... I know that all of you are good chemists ... and I hope I'm good too ... but I'm certainly not the best one ...
Wack, please, the next time you will pick on somebody to haggle him, be more patient, just to see if him really worth to be argued...
And, Zyklonb ...a lot of thank's for that link ... is very useful to me.
Now I can make a lot of N2O5 in a shorter amount of time. And I need just a few grams of Ag...that's easy 
Also I'm wondering if I can use mercury nitrate instead of silver nitrate ... I will test that...
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Ascaridole
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Yay for the P2O5 method!
Just dissolve the P2O5 into some phosphoric acid, yes it will turn some of the P2O5 into phosphoric acid but its much much safer than pouring the
aqueous acid onto P2O5 directly. Use enough P2O5 and I think you will make NO2.... damn P2O5 just wants water I guess...
Ascaridole, the masked bandit of chemistry!
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sesmd
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EASY NITRIC ACID
Quote: Originally posted by gdflp  | | There is an azeotrope of nitric acid with water at 70%, so you will need a vacuum distillation to get nearly anhydrous acid. You will also probably
have to distill it more than once. |
Nitric acid production - potassium nitrate (1 M) + H2SO4 (1 M) in distillation setup. Use CaCl2 trap to exclude moisture. Distill until
no more liquid comes across. This is essentially white fuming nitric
acid. After sitting a few days, NO2 will accumulate -> red fuming acid.
Using equimolar amounts keeps product very nearly anhydrous, as H2SO4
is twice amount actually needed . This does not have large amounts of
free nitrogen oxides, however, seems to work quite well in any prep
calling for 'fuming nitric acid'.
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sesmd
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More on nitric acid..... if one wishes to make nitric acid from easily bought starting materials, the following is very easy.
Basis: Ammonia can be oxidized to nitric oxide (NO) quite readily by passing ammonia + air (or O2) over copper, heated
to a dull red heat. NO produced mixed w/ more air -> NO2 -> +water -> nitric acid (+ more NO, which can be recirculated).
I 'Y' ed together ammonia + air, then passed mixture into 0.25 inch copper tubing, in which I had stuffed an 18 inch length
with BARE fine (34 ga.) copper wire. Purpose was to create reasonably large copper surface area. The 'stuffed' part of the
copper tubing was coiled with 2 ft. straight tails at each end. Coiled part placed in metal can, containing charcoal that had
been ignited and was glowing a dull red. This effectively heated copper tubing. Output end of Cu tubing connected to flexible
plastic tubing -> bubbler in a 100 ml beaker. I ran this until I had yellow appearing liquid present, then distilled to obtain
azeotropic nitric acid containing about 68% HNO3.
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WGTR
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I'm sure that I'm the only person responding so far, because no one else has managed to pick themselves off the floor yet. That's a pretty cool setup
(your second post).
So...what was the yield? Did you take pictures/video/etc.? What type of plastic tubing did you use? How did you keep from melting the plastic
tubing? Did you have trouble with the copper tubing oxidizing? Did you need to allow time for the NO to react to form NO2? How was your
ammonia prepared? Was it anhydrous, etc.?
I managed to fill a bottle with NO from a reactor, but I noticed that it takes at least a couple of minutes to fully form NO2 after the
gasses have cooled down. Reacting the NO2 with water produces more NO, which takes even more time to form NO2...you get the
idea.
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Molecular Manipulations
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Condense N2O4 to a liquid. Add it to water, it will sink to the bottom, then bubble oxygen or dry air into the solution through
both the N2O4 and the water/dilute nitric acid. 99% HNO3 can be produced this way.
The overall reaction is:
N2O4 + H2O + .5 O2 → 2 HNO3
This is ideal because it doesn't allow NO to be formed.
Refs for everything I've posted can be found in Absorption Of Nitrous Gases.
| Quote: |
When liquid nitrogen tetroxide is added to a small quantity
of water a separation into two layers occurs. The upper
layer consists of nitric acid containing dissolved nitrogen
tetroxide, while the lower bluish-green layer consists mainly
of nitrogen trioxide
2N8O« + H2O :;::^N2O3 + 2HN0, .
If, however, oxygen is bubbled through the mixture, the
latter assumes an orange-yellow colour and the tipper layer
is found to contain nitric acid of 95-99 per cent. HNOa—
while the lower lay
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-The manipulator
We are all here on earth to help others; what on earth the others are here for I don't know. -W. H. Auden
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WGTR
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Thanks, that's an interesting link. After reading through it, I can see that NO oxidises faster in air as its concentration goes up.
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annaandherdad
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MM that equation you quote is hard to read, and it's hard to read in the book, too. It looks to me like it should be
2N2O4 + H20 <-> N2O3 + 2HNO3
What should be N2O3 looks like N2O4 in the book, which can't be right. So the lower layer turns blue because of this reaction. I wonder what a
"small amount of water" means, I mean, I wonder if you can make stoichiometric amounts of HNO3 this way.
It sounds simple to do, and I wonder if it could be a useful way to make nitric acid (concentrated at that). The standard procedure of using H2SO4
plus nitrates requires all glass equipment and messing with hot H2SO4. NaNO2, which could be used as a source of NO2+NO, costs $5/lb on ebay.
This is indeed an interesting book, I've been looking at it on and off for some time.
Any other SF Bay chemists?
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Molecular Manipulations
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Yeah the format is strange. It looks fine on my computer but not my phone.
The reaction is this:
N2O4 + 1/2 H2O --> HNO3 + 1/2 N2O3
Then:
N2O3 + H2O + O2 --> 2 HNO3.
Cancel out the intermediates and those shown twice and you get the condensed reaction I posted above.
Despite me wanting to do the reaction again I've only tried it once, got 94% IIRC.
I do have quite a lot of sodium nitrite so I should give it another go sometime soon.
Let me know if you try it. Distillation of a nitrate salt and sulfuric acid is just so easy it makes this seem like a waist.
[Edited on 8-5-2015 by Molecular Manipulations]
-The manipulator
We are all here on earth to help others; what on earth the others are here for I don't know. -W. H. Auden
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annaandherdad
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I'm going to try it, but I'm waiting to receive my NaNO2 from ebay. It's very slow delivery, and I'm getting impatient. This should be fun. I've
been inspired somewhat also by woelen's video on the NO+O2 reaction. I may get some kids involved, we'll be careful.
Any other SF Bay chemists?
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Dan Vizine
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| Quote: Originally posted by Molecular Manipulations |
................
Let me know if you try it. Distillation of a nitrate salt and sulfuric acid is just so easy it makes this seem like a waist.
[Edited on 8-5-2015 by Molecular Manipulations] |
In fact, that is so true that long ago the U.S. military used to have a publication describing that as the first step in manufacturing improvised
explosives, for soldiers/agents caught behind enemy lines. It's foolproof and starts with easily obtained materials. It doesn't get any better than
that.
"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They
Deserve"...F. Zappa
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ave369
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This morning I did a modified version of distilling nitrate salts with an acid. Right now I don't have any concentrated sulfuric acid in stock, only
36%. So I used phosphoric acid, which I have quite concentrated. And guess what? Phosphoric acid works, too, it's a passable substitute for sulfuric
acid.
The nitric acid I've synthesized was quite concentrated, it reacted with copper with "the fox's tail" (NO2) forming.
Smells like ammonia....
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howtomake
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Brother of A look at Vogel Analytical Chemistry, there is a Chapter What if a Refre the reactivity of the groups. The table will display the next
periodic Cu, Ag, Au and Rg this is the copper group, in most cases reactions that occur with copper occur with other but in terms of reactivity can
vary the reaction kinetics ok? silver necklaces are usually black with time, this is to be formed on the surface of silver sulphate on the surface, to
a silver chain be eroded it would take years then it may be very time consuming its reaction with sulfuric acid despite being a strong acid a
reactivity and slow dissociation to have two stages. I believe that the nitric acid and the preferred as being more practical,it reduces reduces
hydrogen, formano silver nitrate 100% soluble in water, in sequence with hydrochloric acid to precipitate silver chloride having the solution again
pure nitric acid in the solution with the sulfate do not know how would have to do the math to indicate that the viability peace.
My inglish is suck
[Edited on 12-9-2015 by howtomake]
[Edited on 12-9-2015 by howtomake]
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NitratedKittens
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This video is a simple way to prepare nitric acid
https://www.youtube.com/watch?v=KBeo8nww21g
And then turn it into silver nitrate
https://www.youtube.com/watch?v=EruzAVv2Odc
Basket of kittens for you ........BOOM
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clearly_not_atara
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"Is it possible to dissolve silver without HNO3?"
It's easier than you ever thought possible:
https://www.researchgate.net/publication/304837924_A_study_o...
Not sure what to do about the presumably silver sulfate byproduct but IIRC silver sulfate is soluble in dilute sulfuric acid (silver bisulfate?) so
you may end with a soluble if acidic salt mixture.
Enough to make silver acetate or tosylate methinks.
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gdflp
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Thread Split
18-6-2017 at 07:32 |
clearly_not_atara
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It turns out that silver methanesulfonate is many times more soluble than the tosylate. This paper quotes the aqueous solubility of
AgOMs as 3.72 mol/dm^3 = 609 g / L, which is far higher than the sulfamate or lactate (and also more than 100x as soluble as
the tosylate), and probably blows oxamate out of the water as well.
Attachment: gernon1999.pdf (290kB)
This file has been downloaded 2071 times
| Quote: | To 500 g of 70% MSA (aq, 3.64 mol) in a 1 gallon beaker, 402 gof silver oxide (3.47 mol of Ag+) was slowly added over 30 min so as to form a uniform
suspension. The temperature of the reaction mixture rose to ca.60°C during the addition, and this temperature was maintained with heating for an
additional 4 h. Thereaction mixture was filtered through a thick 1 mm glassmicrofiber pad, and the filtrate was stripped in vacuo(4 mmHg) to
a solid residue. The solid residue was washed with isopropyl
alcohol and ether. Finally the crystalline product was reduced to constant weight in vacuo(1 mmHg). Theoretical yield = 704 g, actual yield = 450 g
(64%). For Ag(OMs); %Ag/%S (theoretical) = 3.36, %Ag/%S (actual) = 3.37. |
[Edited on 23-7-2017 by clearly_not_atara]
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AJKOER
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No need for any acid to make dilute HNO3 with a few easy steps from cheap available chemicals.
First, mix up a concentrated solution of MgSO4 (Epsom salt) with KNO3 (EDIT: not a hydrate, that is my NaHSO4.H2O) from stump remover. Freeze till
the K2SO4 formation is evident. Decant removing K2SO4, dilute and refreeze to obtain Mg(NO3)2•6H2O. Remove crystals, heat and collect vapors of
dilute HNO3. Reactions:
MgSO4 + 2 KNO3 --> Mg(NO3)2 + K2SO4
Mg(NO3)2 + 6 H2O = Mg(NO3)2•6H2O
Mg(NO3)2•6H2O --heat to over 130 C--> Mg(OH)NO3 + HNO3 + 5H2O
Per a source (https://chemiday.com/en/reaction/3-1-0-7303 ), to quote:
“The thermal decomposition of hexahydrate nitrate magnesium to produce magnesium hydroxide-nitrate, nitric acid and water. This reaction takes
place at a temperature of over 130°C.”
Interestingly, Wikipedia presents an alternate path on the thermal decomposition of magnesium nitrate, likely not referring to the hydrate:
2 Mg(NO3)2 → 2 MgO + 4 NO2 + O2
Reference: see https://en.wikipedia.org/wiki/Magnesium_nitrate
Note, my personal experience, as reported on SM, extends to aqueous Mg(NO3)2 preparation, and once on evaporation upon standing in air, the creation
of a very hygroscopic salt. As such, I doubt if there is an easy path to anhydrous magnesium nitrate, other than discussed below involving NO2, so the
Wikipedia path to NO2 appears circular in all likelihood.
------------------------------------------------------------
Interestingly, in my opinion, dilute nitric acid can be used for nitrating purposes as the nitrate radical is likely more chemically active than even
the strong acid! Just take dilute HNO3 and add a hydroxyl radical source, say N2O in UV light or just UV on nitric acid:
HONO2 + UV = .OH + .NO2
N2O + UV = N2 + .O
.O + H2O = .OH + OH-
NO3- + .OH = .NO3 + OH-
Or, with nitric acid: .OH + HNO3 = H2O + .NO3 (see http://adsabs.harvard.edu/abs/2001JGR...106.4995P )
For further details of subsequent reactions of .NO3 with .OH and .HO2, please see http://pubs.acs.org/doi/abs/10.1021/j100319a029?journalCode=... .
Sample run based on the UV photolysis of methanol and water in the presence of HNO3 to create some methyl nitrate (properties: see https://en.wikipedia.org/wiki/Methyl_nitrate ):
CH3OH + UV = .CH3 + .OH
.OH + HNO3 = H2O + .NO3
.CH3 + .NO3 = CH3NO3
For other possible products, see general discussion at https://books.google.com/books?id=qmsoDwAAQBAJ&pg=PA113&...
Other paths would involve concentrating the dilute nitric acid to the extent that a reaction with copper metal produces NO2 gas, or collecting the NO
from the action of Cu on dilute HNO3 and reacting with O2 to create NO2. To quote from Atomistry.com (link: http://nitrogen.atomistry.com/nitric_oxide.html ):
"When the proportions of nitric oxide and oxygen are as 2:1, the N2O3 stage is reached very rapidly, then further oxidation to N2O4 occurs, 34 per
cent, in 20 seconds, and completely in 100 seconds."
Then, one can just use the stable radical nitrogen dioxide directly, on say, metal oxides to produce anhydrous nitrates. Per Wikipedia on NO2, to
quote:
"Conversion to nitrates
NO2 is used to generate anhydrous metal nitrates from the oxides:[9]
MO + 3 NO2 → M(NO3)2 + NO "
Link: https://en.wikipedia.org/wiki/Nitrogen_dioxide
Apparently, as I recall reported once, the need to avoid rubber joints on boiling HNO3 inspired someone to use aluminum foil that became covered with
anhydrous aluminum nitrate (see http://www.sciencemadness.org/talk/viewthread.php?tid=22790) .
| Quote: Originally posted by Antiswat |
[/rquote]
What I found interesting was that anhydrous aluminum nitrate can be prepared from AlCl3 in N2O4 at 0 °C.
[Edited on 23-12-2012 by AndersHoveland][/rquote]
A bit off topic, but when ive made Pb(NO3)2 by HNO3 + Pb i have covered my flask with 10 layers of aluminium foil, and apparently the NO2 formed can
and WILL react with the aluminium foil to make aluminium nitrate, infact this reaction is probably taking place right now, just thought its weird that
aluminium wont react with HNO3 but NO2 reacts with aluminium |
[Edited on 10-12-2017 by AJKOER]
[Edited on 10-12-2017 by AJKOER]
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JJay
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I hadn't seen nitric acid since high school until I made some yesterday, and I feel like a complete newb on this particular topic, but do you have a
reference stating that stump remover is potassium nitrate monohydrate? I had thought it was anhydrous....
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clearly_not_atara
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Saltpeter does not form a monohydrate: | Quote: | | It is not very hygroscopic, absorbing about 0.03% water in 80% relative humidity over 50 days. |
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AJKOER
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I was probably confused by my NaHSO4.H2O, which does exist! See http://www.endmemo.com/chem/compound/nahso4h2o.php .
However, at times, I just feel that my stumper remover source of nitrate may not be 100%, interestingly a search on KNO3 does suggest a brand
preference,
Will edit nevertheless.
----------------------------------------------
Did find a good review on the nitrate radical, for those interested, see https://ac.els-cdn.com/096016869190192A/1-s2.0-0960168691901... .
The source outlined some new reactions for me which could result in the nitrate radical creation, like:
.NO2 + .HO2= NO2HO2 --> .NO3 + .HO
.NO2 + .RO2 = NO2RO2 --> .NO3 + .RO
[Edited on 11-12-2017 by AJKOER]
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AJKOER
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Yet another possible (?, the literature is not entirely clear) with a seemingly simple and available path to dilute HNO3.
Per a source (http://www.societechimiquedefrance.fr/extras/Guiochon%20VO/d... ) to quote:
"Chloride ions catalyze another decomposition reaction:
5 NH4NO3 ----> 4 N2 + 2 HNO3 + 9 H2O "
So, a possible process could be first, mix up a concentrated solution of MgSO4 (Epsom salt) with KNO3 available as stump remover. Freeze till the
K2SO4 formation is evident. Decant the aqueous Mg(NO3)2 removing the K2SO4 hydrate. Add ammonia water obtaining a white suspension of Mg(OH)2 in
aqueous NH4NO3. Filter out the magnesium hydroxide or just let settle (in days) and decant. Let the solution evaporate leaving NH4NO3. Add an equal
amount of say NH4Cl (see Fig 4 at https://www.researchgate.net/publication/263578419_Review_on...) or perhaps Cl2 (but not in excess of created NH3 or existing NH4+ so as to avoid
NCl3) and water vapor or just NaCl (see https://aip.scitation.org/doi/abs/10.1063/1.1733343 ?) and, with a blast shield in place, gently heating the (dry or wet?) powder mix condensing
the vapors of dilute HNO3.
Does anyone have more info on this process (like temperature) and a confirming source on the chloride catalyze decomposition reaction with NH4NO3?
Here is a source (see https://pubs.acs.org/doi/abs/10.1021/ja971618k?journalCode=j... ) describing an acid + chloride path in aqueous conditions at 180 C. A possibly
conflicting reporting where the added acid cited is aqueous HNO3 with a product only of N2O at 100 C at https://www.sciencedirect.com/science/article/pii/0022190279... .
--------------------------------------
My best speculated path to nitric acid is for a slow and very low temperature heating (to the point of sublimation) of dry NH4NO3 in the presence of
dry chlorine gas (not in excess):
8 NH4NO3 + Low heat --> 8 NH3 + 8 HNO3
8 NH3 + 3 Cl2 --> 6 NH4Cl + N2
Net: 8 NH4NO3 + 3 Cl2 --> 6 NH4Cl + N2 + 8 HNO3
So, for example, per above 4 grams of ammonium nitrate could be slowly heated in 420 cc of dry chlorine creating possibly 2 cc of HNO3, 2 grams of
NH4Cl and 140 cc of nitrogen, by my calculations.
------------------------------------------------------------------
Note, as I previously performed on SM, chlorine gas can be sourced from a 'bleach battery' without the use of a strong acid. Here is a detailed
rehash of the steps involved in the so called Bleach battery:
1. Whip up some Hypochlorous acid by mixing bleach (NaOCl) and vinegar (which contains Acetic acid HAc) in the volume ratio 1.4 parts of 5% vinegar to
one part of 8.25% extra strength chlorine bleach.
2. To the HOCl add a piece of copper metal which will function as the cathode and an Aluminum source (like foil, but heat to red on a stove to
increase reactivity) to act as the anode.
3. Lastly, add much NaCl to act as the electrolyte and to salt out the chlorine. I usually jump start the reaction in a microwave (1 minute should
work).
The underlying chemical reaction leading to hypochlorous acid is given by:
NaOCl + HAc --> HOCl + NaAC
-------------
An alternate preparation of HOCl creating more conc HOCl (which is also avoids organic acids subject to attack by the hypochlorous acid in the
presence of copper) is:
2 NaOCl + CaCl2 = 2 NaCl + Ca(OCl)2
Ca(OCl)2 + 2 NaHCO3 --> Na2CO3 + CaCO3 (s) + 2 HOCl (cool and let stand to remove the CaCO3)
Net: 2 NaOCl + CaCl2 + 2 NaHCO3 --> 2 NaCl + Na2CO3 + CaCO3 (s) + 2 HOCl
------------------------
My take on the major electrochemical half-reactions:
In anodic zone (aluminum pieces):
6 H2O <--> 3 H3O+ + 3 OH-
Al + 3OH- ⇒ Al(OH)3 + 3 e-
At the cathode (copper metal):
3 HOCl + 3 H3O+ + 3 e- ⇒ 3/2 Cl2(g) + 6 H2O
for an implied net reaction of:
3 HOCl (aq) + Al (s) --NaCl--> Al(OH)3 (s) + 3/2 Cl2 (g) Eo net = 3.93 V
Note, the moles of consumed HOCl (from NaOCl) to form one mole is not as efficient as employing, for example, NaHSO4 acting on NaOCl+NaCl, but no
strong acid or acid salt was used!
Incidentally, the battery cell is theoretically capable of generating 3.93 volts. References: see http://www.exo.net/~pauld/saltwater/ and http://sci-toys.com/scitoys/scitoys/echem/batteries/batterie... and also http://www.dtic.mil/dtic/tr/fulltext/u2/d019917.pdf
[Edited on 9-7-2018 by AJKOER]
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AJKOER
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On the above heating of NH4NO3 and Cl2, I would stress, it is potentially a more dangerous path! I would strongly advise to either gradually
introduced the chlorine gas, or the NH4NO3 should be heated (in small amounts only between 170 C and 190 C) over a large flat surface so as to reduce
the likelihood of high local concentrations of Cl2 versus NH3 (and any subsequent NCl3 creation).
Water/water vapor should be avoided, in my opinion, also for a possible safety concern. My logic is:
Cl2 + H2O = HCl + HOCl
3 HOCl --> 2 HCl + HClO3
NH3 + HClO3 --> NH4ClO3
where, if created, the ammonium chlorate could very likely explode and act to detonate also the NH4NO3.
So, small quantities and a safety blast shield required!
[Edited on 9-7-2018 by AJKOER]
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