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good product with poor shelf life

Posted on Poppers Guide's Forum

Topic created by The Professor
on Tue, 10 Aug 2021 at 21:34

The Professor said on Tue, 10 Aug 2021 at 21:34...

One thing has has been a nuisance to some makers is that they have a good outcome from the preparation, but the product decomposes very fast, even with stabilizers added.

In almost every case, this can be attributed to a failure in the drying process.

The drying process can be of liquid-liquid extraction (typically a wash with brine followed by a drying agent such as magnesium sulphate). This is a rather crude drying agent, and will be suitable for in situ preparations, but leaves quite a few water molecules in the nitrite.

Adsorption is another method, and it can have superior performance as compared to liquid-liquid extractions, but it takes more time,

The following will give you a nitrite that is dry within 15 parts per million (ppm), and that will stabilize nicely (at least 3 months unopened)

After preparation, I have been skipping the wash/dry step and only neutralizing.

Neutralizing itself will kill of some of the yield if done properly (some makers just add sodium bicarbonate (baking soda) to the crude yield, watch it fizz a tiny bit, and call it good.

This is NOT good; it is why most of the OTC stuff burns your throat or nostrils, stuffs up your nose, raspy throat, etc.

To properly neutralize the excess acid that is dissolved in the yield you need to first at 20% w/v of distilled water, then 20% w/v baking soda and stir or shake until no longer fizzing. If you have a magnetic stir bar, set it on high speed and slowly sprinkle in the baking soda. Remove the water layer on the bottom and proceed.

That's a neutralization, quick, easy, and it can also be used to quickly remove acids from a putrid OTC product. It won't eliminate the resulting SALTS (e.g. neutralizing butyric acid leaves behind sodium butyrate), but it will remove many objectionable qualities of an otherwise 'dead' bottle.

But, back to the point.

AFTER your nitrite is neutralized, and if you don't intend to use it right away, instead of wasting nitrite with the traditional drying method, try 3 angstrom molecular sieve.

At 20% w/v, MS3 left under the yield for 96 hours will give you a product that is dry within 20ppm; that's EXTREMELY dry. I typically use a stoppered 125ml Erlenmeyer flask.

Those 4 days are the beginning of my 22 day 'proof of concept' post processing routine, and it is proven to result in a product that's suitable for stabilization.

Anonymous said on Wed, 11 Aug 2021 at 02:08...

Why sprinkle vs making up an bicarb solution then agitating w/ crude?

Isn't the end result of the hydroxide w/ the crude the same w/o the fizzle?

Is the fizzle desirable?

Maxed out 3 ques - Thanks

Kmo said on Wed, 11 Aug 2021 at 07:49...

Need rush 10ml

The Professor said on Wed, 11 Aug 2021 at 16:11...

@Anonymous:
The desired effect is too neutralize acid dissolved in nitrite. This can be done in many ways, but an inexpensive and likely compounds is baking soda (NaHCO3).

Acid +base = a salt + water.

In this case, as a bonus, NaHCO3 also liberates CO2.

e. g. HCL + NaHCO3 = NaCl + H2O + CO2

The end of CO2 liberation is an indicator that the neutralization had completed.

One can implement this in any fashion that they desire; I'm just relaxing a method that works quite effectively to pull dissolved acid out of a nitrite. Nitrite isn't water soluble, just dumpling bicarb into it won't work; I mention this in the original post.

Anonymous said on Thu, 12 Aug 2021 at 03:23...

Prof, Thanks for the tap and dance.

The Professor said on Thu, 12 Aug 2021 at 18:39...

@Anonymous:
no problem, you're a prince among kings.

TL;DR

if you're a maker, this step is critical to a customer's experience.
If you're a customer, this can recover a nasty product.

Jacko said on Sun, 29 Aug 2021 at 03:34...

Thanks, @TheProfessor. To date I've made a separate slurry of bicarbonate and pure water, then agitated this at high stir speed with the crude decanted nitrite immediately after removing the brine. Is there any reason why dry bicarbonate addition is preferable to making and emulsion and allowing it to layer out again?

The Professor said on Sun, 29 Aug 2021 at 19:20...

@Jacko:

Any routine that pulls the acid that is dissolved into the nitrite will work; the main point being that manufacturers that THINK that they are neutralizing by just adding baking soda (no water) are leaving quite a bit of dissolved acid which will cause sore throat, congestion and acrid Aromas.

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