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PHILOU Zrealone
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Quote: Originally posted by Hexogen  | I understand the instability of Armstrong's mixture due to it composing of a strong oxidizer and red phosphorous.
Would it be possible to set off a mix of 9:1 mix of KClO3 and PIB
(Polyisobutylene) ? |
Not only that explaination...
Red P is a reducing stuff (thus a fuel for the oxidizer).
Red P is so reducing that it reacts superficially to make some P2O5 (at a lower speed than white P)... the later turns into H3PO4 from air moisture...
acids are uncompatible with chlorates since they set HClO3 free and explosive ClO2.
Also P2O5 may set directly very reactive (explosive) Cl2O5 free out of the chlorate...
The PIB/chlorate (KClO3) initiation has already been discussed a few days ago
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Hexogen
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| Quote: Originally posted by PHILOU Zrealone | | Quote: Originally posted by Hexogen | I understand the instability of Armstrong's mixture due to it composing of a strong oxidizer and red phosphorous.
Would it be possible to set off a mix of 9:1 mix of KClO3 and PIB
(Polyisobutylene) ? |
Not only that explaination...
Red P is a reducing stuff (thus a fuel for the oxidizer).
Red P is so reducing that it reacts superficially to make some P2O5 (at a lower speed than white P)... the later turns into H3PO4 from air moisture...
acids are incompatible with chlorates since they set HClO3 free and explosive ClO2.
Also P2O5 may set directly very reactive (explosive) Cl2O5 free out of the chlorate...
The PIB/chlorate (KClO3) initiation has already been discussed a few days ago |
Ah I see, I overlooked the underlying reactions that may occur with the red phosphorus.
Anyway I plan to synthesize a small amount (<15g) of HMTD which I plan to use as the primary ASAP when I prepare the Cheddite C.
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kratomiter
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15 g HMTD, even 10 g, is not a small amount. It is enough to detonate even unconfined.
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Hexogen
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That's just a theoretical amount, since I hope to only use it for a blasting cap.
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Bert
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Say hi to Phone for us when you meet him.
| Quote: | Originally posted by Bismuth
||
|| Phone's post before he killed himself that weekend are definitely on the E&W archive. See "Storing the AP" on the archive and you'll see his
post...
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|| ===========================================
|| phone
|| February 21st, 2004, 07:08 AM
|| i wonder if in europe there is anyone that uses mehenamine for fire tablets or other things..i found only petrol derivate tablets...
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|| Yeah. They´re german, I don´t have the pack right here, but it´s almost pure methanamine (or how you now spell that lame word). You just solve
it in aceton and you get it pure (or was it water) I haven´t really memorized it since I am an AP lamer (but I do own a pack with methanamine), HMTD
is nutting for me  , but hey, first time I did AP I did 80 grams, second 120
grams, third time (yesterday, drying today) something about a kilo or more... I
GONNA BLOW MY FRICKING ARMS OFF! And yeah, I don´t treat AP with respect, but well, I got plenty of cold, snow and ice outside so my AP is usually
quite resistant against pressure e.tc. Well, right now my brain feels like weird, I gonna have to put up a few lamps e.tc. (it dried overnight,
switched the newsspaper it was on) and I think I gonna put up a few lamps to get the bitch dry faster. Well, my moms out of the weekend, that´s why I
am sitting here with over 1 kilo AP and lots and lots and lots AN. Well, sure, I spam... but.. hey! Well.
||
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|| Well, almost forgot, I always take all my explosives and just make 1 big fucking bomb of it. 1 kilo AP and a couple of kílos AN coming up.
|| ===========================================
||
|| Now, that was Feb 21st. Now we look at this thread posted on Feb 22nd:
|| http://www.sciencemadness.org/talk/viewthread.php?tid=1570 |
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hexogen
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| Quote: Originally posted by Bert | Say hi to Phone for us when you meet him.
| Quote: | Originally posted by Bismuth
||
|| Phone's post before he killed himself that weekend are definitely on the E&W archive. See "Storing the AP" on the archive and you'll see his
post...
||
|| ===========================================
|| phone
|| February 21st, 2004, 07:08 AM
|| i wonder if in europe there is anyone that uses mehenamine for fire tablets or other things..i found only petrol derivate tablets...
||
||
|| Yeah. They´re german, I don´t have the pack right here, but it´s almost pure methanamine (or how you now spell that lame word). You just solve
it in aceton and you get it pure (or was it water) I haven´t really memorized it since I am an AP lamer (but I do own a pack with methanamine), HMTD
is nutting for me , but hey, first time I did AP I did 80 grams, second 120
grams, third time (yesterday, drying today) something about a kilo or more... I
GONNA BLOW MY FRICKING ARMS OFF! And yeah, I don´t treat AP with respect, but well, I got plenty of cold, snow and ice outside so my AP is usually
quite resistant against pressure e.tc. Well, right now my brain feels like weird, I gonna have to put up a few lamps e.tc. (it dried overnight,
switched the newsspaper it was on) and I think I gonna put up a few lamps to get the bitch dry faster. Well, my moms out of the weekend, that´s why I
am sitting here with over 1 kilo AP and lots and lots and lots AN. Well, sure, I spam... but.. hey! Well.
||
||
|| Well, almost forgot, I always take all my explosives and just make 1 big fucking bomb of it. 1 kilo AP and a couple of kílos AN coming up.
|| ===========================================
||
|| Now, that was Feb 21st. Now we look at this thread posted on Feb 22nd:
|| http://www.sciencemadness.org/talk/viewthread.php?tid=1570 |
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Why was he making large amounts of a primary explosive ?
Why was he making TATP ?
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Bert
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Phone.
He was a kid, not an especially thoughtful one, who wanted to hear a big BANG. Then he was a dead kid, scattered over the snow in his local park in
Sweden, because he went back to a charge after fire had been applied, as he was both ignorant and impatient (he thought it had failed. It had not...)
At least he did not kill his friends or the neighbors in his mother's apartment building.
I responded to that post, probably in the last couple of hours he was alive. Still regret what I wrote, and wish I could have written something to
make him see how dangerous what was doing was instead. Some people just can not learn safety any way but by peeing on an electric fence for
themselves. Are you one of them?
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hexogen
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| Quote: Originally posted by Bert | Phone.
He was a kid, not an especially thoughtful one, who wanted to hear a big BANG. Then he was a dead kid, scattered over the snow in his local park in
Sweden, because he went back to a charge after fire had been applied, as he was both ignorant and impatient (he thought it had failed. It had not...)
At least he did not kill his friends or the neighbors in his mother's apartment building.
I responded to that post, probably in the last couple of hours he was alive. Still regret what I wrote, and wish I could have written something to
make him see how dangerous what was doing was instead. Some people just can not learn safety any way but by peeing on an electric fence for
themselves. Are you one of them? |
I am fully aware of anything that can go wrong (Murphy's law) and is why you cannot skip on PPE and some common sense.
If I wanted to hear a bang, a firecracker would do.
Chemistry is love, chemistry is life.
I have done fireworks before (nothing compared to the power of EM) where people think it's failed only to get almost deafened.
Thank you for bringing this up as it might be sensitive too you, since you may think it's your fault.
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PHILOU Zrealone
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Love of chemistry and love of life is good  ... but careless love of chemistry can
be lethal 
Maybe that he was too enthousiastic about his first succes... and thought he masterizes the stuff and its inherent dangers...
Also the fact he was in a demo mode (kind of braging in front of his friend) didn't help...
==> he was less cautious and careless... then he faced his own death.
Just to ear a good bang... no need for 80g, 120g or 1kg+ CTAP nor to risk
someone's life...
Edit:
Peroxides are sensitives bitches, HMTD even more so than CTAP...
Playing with it in large amounts is suicidal... even tiny amounts can cause injuries... cristalline stress during cristallization due to an error into
the cristal lattice may cause premature detonation under the slightest pressure/friction.
So sometimes it is relatively stable and doesn't cause troubles during handling... but once in a while it does... there are countless reports of those
incidents.
[Edited on 18-10-2017 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Bert
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| Quote: |
I am fully aware of anything that can go wrong
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Nope.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hexogen
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Everything will go wrong.
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nitro-genes
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The selective reduction of a single nitro group for polynitro arenes is usually performed by the still poorly understood zinin reaction using
sulfides. However, according to these papers (1,2): a single nitro group can actually be reduced in high yield using nascent hydrogen under anhydrous
conditions.
How can the presence of water make this reaction that much more aspecific? Is it because nitronates form in presence of water and are more easily
reduced? How detrimental would only a few percent of water in the reaction be?
(1) Atkins, Ronald L., and William S. Wilson. "Synthesis of polynitrodiazophenols." The Journal of Organic Chemistry 51.13 (1986): 2572-2578.
(2) Anschütz, Richard, and Fritz Heusler. "Ueber die schrittweise Amidirung von mehrfach nitrirten aromatischen Substanzen mittelst Zinnchlorür."
European Journal of Inorganic Chemistry 19.2 (1886): 2161-2162.
[Edited on 31-10-2017 by nitro-genes]
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PHILOU Zrealone
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| Quote: Originally posted by nitro-genes | The selective reduction of a single nitro group for polynitro arenes is usually performed by the still poorly understood zinin reaction using
sulfides. However, according to these papers (1,2): a single nitro group can actually be reduced in high yield using nascent hydrogen under anhydrous
conditions.
How can the presence of water make this reaction that much more aspecific? Is it because nitronates form in presence of water and are more easily
reduced? How detrimental would only a few percent of water in the reaction be?
(1) Atkins, Ronald L., and William S. Wilson. "Synthesis of polynitrodiazophenols." The Journal of Organic Chemistry 51.13 (1986): 2572-2578.
(2) Anschütz, Richard, and Fritz Heusler. "Ueber die schrittweise Amidirung von mehrfach nitrirten aromatischen Substanzen mittelst Zinnchlorür."
European Journal of Inorganic Chemistry 19.2 (1886): 2161-2162.
[Edited on 31-10-2017 by nitro-genes] |
Can you provide me the documents or links to download them?
Thank you in advance for this.
The funny thing is that nascent hydrogen usually refers to naked metal into an acidic media (usually containing water)...
Typical examples of organic chemistry are Zn/HCl, Mg/AcOH,... or Fe/HCl.
I wonder what is their specific anhydrous reduction system?
Zn into glacial AcOH (what is anhydrous)?
Into organic chemistry the solvent/mix of solvents usually pay an important role.
It may favourize certain reaction pathways over others by lowering the general activation energy or lowering one of the intermediary energy "hills"...
you may see it as a kind of catalyst or stabilisator of intermediary unstable molecules.
==> There is a change in the speed of reaction/reaction kinetic
So it is a matter of statistic (induced by the different reaction pathway kinetics)...if the water is a strong perturbator of the reaction pathway;
then a little will induce a heavy change of composition; if not then % water will have little impact and the process modification will be still good
despite a few % water and modification could be smoother.
Water will have a marked influence onto the pH and dissociation constant of the acid/bases/salts... this also has an impact onto many
reactions...addition or elimination of H(+) or of OH(-)...etc.
[Edited on 31-10-2017 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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nitro-genes
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Thanks Philou, its an interesting question what determines the selectivity of the reductions, not only regarding the number of nitro groups attacked,
but also the position seems dependent on solvent, pH and reducer utilized. In
the first article a single ortho nitrogroup of TNT is reduced using Fe(0)/AcOH, in the second mentions 2,4 dinitrotoluene reduction to 2-amino 4
nitrotoluene using either tin/HCl/ethanol or ethanol/anhydrous tin(II)chloride. The second article also mentions that Kekule explained in detail in
one of his learning books how the presence of water leads to attack of all nitro groups simultaneously (Band II, S. 519), which made me curious what
this precise reason is.
Attachment: Synthesis of Polynitrodiazophenols.pdf (834kB)
This file has been downloaded 581 times
Attachment: php0wFAMH (104kB)
This file has been downloaded 504 times
[Edited on 31-10-2017 by nitro-genes]
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kratomiter
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Methylamine perchlorate
I want to make methylamine perchlorate from ammonium perchlorate and paraformaldehyde. I have no experience with paraformaldehyde, can I hydrolize it
in neutral or acid medium? Typical basic medium with NaOH will form NaClO4 and ammonia gas, so it has to be avoided.
Once the formaldehyde solution is made, the reagents will be reacted in a 1:1 mol basis at high temperature.
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ninhydric1
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Heat the paraformaldehyde to decomposition. Formaldehyde gas is produced.
The philosophy of one century is the common sense of the next.
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kratomiter
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I prefer to work with solutions, formaldehyde gas is not very... friendly. I hope heating in neutral medium with methanol to do the trick. Other
trouble is that methylamine perchlorate is very soluble in water so then I have to boil it carefully until precipitation begins.
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PHILOU Zrealone
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| Quote: Originally posted by nitro-genes | Thanks Philou, its an interesting question what determines the selectivity of the reductions, not only regarding the number of nitro groups attacked,
but also the position seems dependent on solvent, pH and reducer utilized. In
the first article a single ortho nitrogroup of TNT is reduced using Fe(0)/AcOH, in the second mentions 2,4 dinitrotoluene reduction to 2-amino 4
nitrotoluene using either tin/HCl/ethanol or ethanol/anhydrous tin(II)chloride. The second article also mentions that Kekule explained in detail in
one of his learning books how the presence of water leads to attack of all nitro groups simultaneously (Band II, S. 519), which made me curious what
this precise reason is.
[Edited on 31-10-2017 by nitro-genes] |
Thank you very interesting documents...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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| Quote: Originally posted by kratomiter | I want to make methylamine perchlorate from ammonium perchlorate and paraformaldehyde. I have no experience with paraformaldehyde, can I hydrolize it
in neutral or acid medium? Typical basic medium with NaOH will form NaClO4 and ammonia gas, so it has to be avoided.
Once the formaldehyde solution is made, the reagents will be reacted in a 1:1 mol basis at high temperature. |
Extremely wrong idea...
The process to make methylamine from hexamine (or NH3/CH2=O) is only safe when the hydrochloride is involved (thus hexamine hydrochloride or
dihydrochloride)... alternatively NH4Cl/formaldehyde or paraformaldehyde heating.
Formaldehyde is unstable in strongly alkaline media like NaOH... it is subjected to a Cannizaro reaction (disproportionation)... this is actually what
happens when methylamine is formed from methylene-imine (discretely hidden into the hexamine)...
CH2=O + CH2=O -base-> CH3OH + HCO2H
CH2=NH + CH2=NH --> CH3-NH2 + HCO2NH4
So formic acid or formiate is formed
The process is strictly forbidden when starting from NH4NO3 and even more so from NH4ClO4...
The all batch may detonate because into the mix in fusion (thus overheated) you have very sensitive hexamine perchlorate/diperchlorate and methylamine
perchlorate.
Risk is a little lower from hexamine nitrate/dinitrate and methylamine nitrate... but stil quite possible if you have a hot spot.
==> De nada... I just saved your life, your glasware and saved you a visit from the police
[Edited on 4-11-2017 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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kratomiter
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Thank you for saving my life xD
But are you talking about heating a solid AP/PFA mix? My initial idea was to hydrolize PFA to make a concentrated formaldehyde solution in neutral or
slightly acidic media, and then add a AP solution and heat, much like is made with ammonium chloride to make methylamine HCl. Is there any risk of
detonation in solution?
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Rosco Bodine
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| Quote: Originally posted by kratomiter | I want to make methylamine perchlorate from ammonium perchlorate and paraformaldehyde. I have no experience with paraformaldehyde, can I hydrolize it
in neutral or acid medium? Typical basic medium with NaOH will form NaClO4 and ammonia gas, so it has to be avoided.
Once the formaldehyde solution is made, the reagents will be reacted in a 1:1 mol basis at high temperature. |
A special method is required for the nitrate and is probably adaptable for the perchlorate but the details are not found reported. The reaction can be
done in aqueous solution with temperature control because the reaction is exothermic and would be scale sensitive and would have safety issues if not
controlled.
Paraformaldehyde can be depolymerized by NaOH in H2O with heating to produce a formaldehyde solution.
Relevant patents for methylamine nitrate are EP0037862 and GB1548827 attached
Probably a much safer method would be to first make methylamine hydrochloride and react with sodium perchlorate.
Attachment: EP0037862 methylamine nitrate.pdf (425kB)
This file has been downloaded 560 times
Attachment: GB1548827 methylamine nitrate related.pdf (320kB)
This file has been downloaded 468 times
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kratomiter
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Thank you for the useful patents! I see that isolating pure methylamine perchlorate will be difficult, maybe I should stick to the well known
guanidine perchlorate or give a try to gel explosives.
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JJay
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What do people typically use for scrubbing nitrogen oxides when making nitric acid? Will sodium carbonate solution work, or do I need something
stronger?
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Cryolite.
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An alkaline water solution would probably work for nitrogen dioxide, but since nitric oxide is so insoluble in water I dont think that sodium
carbonate would do a great job with scrubbing it. You could try urea solution-- the nitrogen oxides oxidize it to nitrogen, water, and carbon dioxide.
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PHILOU Zrealone
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| Quote: Originally posted by JJay | What do people typically use for scrubbing nitrogen oxides when making nitric acid? Will sodium carbonate solution work, or do I need something
stronger?
|
H2O2 and Na2CO3 (or NaHCO3) should prove to be usefull...
The H2O2 will oxydise the NO (colorless) to NO2 (yellow) and the HONO to HONO2 (nitous acid to nitric acid).
2 NO2 + H2O --> HONO2 + HONO
So in fine with NaHCO3 or Na2CO3 you end up with recoverable NaNO3 and H2O and gaseous CO2...
Lately I have used HNO3(69%) and metallic Ag... you get some NxOy...
The use of H2O2 discolored immediately all NxOy color from the liquid reactant, it bubbled some O2 and accelerated a bit the very slow dissolution of
the 99,99% Ag wire.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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