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Some NAN success....

Posted on Poppers Guide's Forum

Topic created by Nitritespecialist
on Mon, 5 Apr 2021 at 16:04

Nitritespecialist said on Mon, 5 Apr 2021 at 16:04...

I have had some success making new NAN brews. It appears that the Blitz, excess acid/SN, method is not necessary to achieve good brews - that it's not a magic bullet. I have made 2 - 20 mls NAN brews using my prior method and they both seem good. The one thing I did that was likely crucial is I pulled my SN from the bottom of my Sigma SN. In theory, the bottom layers are least exposed to air and therefore less degraded. I have also been more aggressive with acid neutralization....using sodium carbonate in addition to baking soda. NaCarb is pH 11.4 and baking soda is 8.4. I am ending up with a very mild, non bitey, non acidic, slightly sweet and fruity, non pungent popper with very pleasant effects. I have stored only on anhydrous Kcarb and it seems effective enough.

Amounts used....30 mls DW plus 24 mls alcohol, chilled, plus 16 grams SN.....moderate to high stir on ice.....dripped in 24 mls cold muriatic. Around 20 mls yield.

Nitritespecialist said on Mon, 5 Apr 2021 at 16:07...

The one telltale sign that the NAN, or any popper is good, is there should be ZERO bitterness to the odor. Even slight traces of bitterness almost always correlate to worse effects.

justChem said on Mon, 5 Apr 2021 at 19:39...

I am using fairly the same ratios SN:alc:acid 1:1.2:1.3
yesterday I made a brew .At the end of the reaction the brew turned green and gave me fumes. That was a singh that the alcohol was finish .
I washed it with sodium bicarbonate but after I added it to water (so it then was just soda) .
Its a common error to add soda or sodium bicarbonate or nacarb etc on a anydrous vesel .If you put the brew on a seperatory vesel and seperate the "durty" NAN ,you cannot just add soda as crystals. they just dot react if the are not in water sulution .

Nitritespecialist said on Tue, 6 Apr 2021 at 15:13...

@JustChem. I had suspected all my reagents as being bad. But I have since ruled out my TCI one pentanol and my Sunnyside muriatic from Menards. I have ruled in my food grade Duda SN as being bad.

I have made 3 - 20 mls brews of NAN successfully using TCI alcohol, muriatic and Sigma SN. Only when I use Duda SN do I get bad results.

I am using water first, then baking soda/brine, then baking soda/sodium carbonate/brine to do a series of cold washes...up to ten...to neutralize. I smell it during the wash cycles to make sure there is no bite and it is smelling fresher. I put a drop of the popper on litmus paper and it showed 6...slightly acidic. I dry on anhydrous mag sulfate and then store on anhydrous Kcarb.

I cover with argon gas, both the SN and finished popper.

Ratios/amounts....30 mls DW and 24-25 mls one pentanol, cold.
16 grams Sigma SN added to this solution.

In a glass flask in ice water, I commence reaction on moderate to high stir, a visible vortex is seen. I drip in ice cold 24-25 mls muriatic acid. I see no green, no blue, no gas, no bubbles....near the end I see a deeper shade of yellow forming near the vortex. I let stand 15 minutes. When I harvest I see a faint yellow layer sitting on top of a slightly cloudy white watery layer. There is mostly stillness. The crude popper smells sour/acidic, until I start washing it.

justChem said on Tue, 6 Apr 2021 at 21:44...

I think you overdue with the washings . Someone mentioned that when NAN is on too much basic solution it tends to degrade too alcoohols and acid again . I think that 3-4 washings (soda -nacl- nacl- anydrus mag of hole day ) is enougth to clean it
I dont know if my SN is clean,but when I melted it to 300C it just conveted to liquid ,without any other kind of particles inside. Then it got rockhard and became dificult to brake it ...
I use HCL which I think its better for this reaction
My major failures was because I was not calculated right the moles of the reaction .I confused grams with mls and ofcourse, all of them went bad ...

justChem said on Tue, 6 Apr 2021 at 21:46...

Thats why I ,now prefer mols for my calculations .

Nitritespecialist said on Wed, 7 Apr 2021 at 22:47...

@JustChem....I am not sure how much to neutralize, but water and acid kill the popper very quickly. I will let time, sitting in the fridge, tell me if I've neutralized my NAN too much. If after a week, I still have a fresh smelling potent popper, then I think I have not been too aggressive with neutralizing.

Nitritespecialist said on Fri, 9 Apr 2021 at 10:12...

None of my most recent 20 mls brews have aged successfully, despite using both MS4, Kcarb and argon. The odors have now all gone flat....smelling like dead wood, all within a week's time.

So I assume that my starting product was not pure enough....that I am not making a pure enough NAN to start with.

N-butyl nitrite is very hard to make as well. It should smell like sweet bananas even as it degrades....the residue will smell like very sweet bananas. I know this for a FACT because I paid $80 for 25 mls of Sigma Aldrich's NBN. So if anyone wants to contest this, please contact Sigma. None of my homebrew NBN has ever smelled like bananas or a locker room, so it's safe to assume it wasn't very pure.

The Professor said on Sun, 11 Apr 2021 at 20:56...

A by-product of preparation called Butyric acid is responsible for the banana, old socks, body odor.

It can easily be avoided during prep

justChem said on Mon, 12 Apr 2021 at 00:30...

@The Professor OK but a solution to the the problem is even better than adress it...

The Professor said on Mon, 12 Apr 2021 at 19:19...

The solution is to either avoid the production of butyric acid, or cull it from the crude nitrite before post processing

Nitritespecialist said on Fri, 16 Apr 2021 at 15:46...

I would think any acids present in a crude popper would be removed or neutralized during the wash/rinse/neutralization steps. Some recommend a neutralization step before distillation as the acid could cross over. Butyric acid smells like sour milk according to Wikipedia. Isoamyl acetate smells like bananas as do several other compounds. The NBN I bought from Sigma had no sort of foul odor, even once degraded to total impotency. It merely smelled like very sweet bananas with the addition of sodium carbonate. Prior to the addition of NaCarb....it was acidic smelling.

The Professor said on Fri, 16 Apr 2021 at 17:49...

isoamyl acetate smells like bananas, yes, and it is a decomp product of isoamyl nitrite. It tends to have a stable aroma at varying concentrations, which is why it's used to test the seals in gas masks (if you can smell banana through it, you have a leak)

Butanoic acid has many aromas at different concentrations; the palate is NOT constrained to 'sour milk'; If you've ever held it in your hands, you'd know that it has various odors. butter, cheese, rancid butter or cheese, body odor, vomit, etc.

Isoamyl acetate can be a decomp of isoamyl nitrite, but isn't present in a pure sample, and is only present in Isoamyl nitrite, not any of the butyls or propyls

Butanoic and propanoic are decomp products of ANY alkyl nitrite

The Professor said on Sat, 24 Apr 2021 at 21:59...

@NitriteSpecialist said
"I would think any acids present in a crude popper would be removed or neutralized during the wash/rinse/neutralization steps."

you'd think wrong.

1. the washing step is actually a liquid-liquid extraction that targets the removal of excess water through a brine solution. It will not remove anything else, just H2O. A different liquid-liquid extraction is required to sequester Butyric acid.

2 the neutralization step will buffer highly acidic liquids like HCL or H2SO4, but will NOT remove butyric; it is a very weak acid to begin with

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