Posted on Poppers Guide's Forum
Topic created by HomeBrewNovice
on Thu, 21 Jul 2022 at 18:56
HomeBrewNovice said on Thu, 21 Jul 2022 at 18:56...
Does anyone know if this method of mixing makes sense and is there anyone to tell when reaction is done and if enough nitrous acid was created?
Place the sodium nitrite in water and add the alcohol. The alcohol will float on top to form a visible layer. Now add the acid below the alcohol layer ONLY with the stir bar on moderate mixing so that the alcohol layer stays mostly on top. When the acid is added, lots of tiny bubbles form and rise up along with a blue color developing. What are the tiny bubbles? Nitric oxide? And will these form the nitrite once they encounter the top layer of alcohol? Also, why would brown gas form? Can this Nitrogen Dioxide gas also combine with alcohol to form the nitrite? I read where nitrogen gases can be blown through alcohol vapor to form the alkyl nitrite. Is the same thing happening in the liquid phase method? When the blue color is mostly gone, is it time to harvest?
Lots of questions, but I don't know the answers. I just know the theory.
The Professor said on Thu, 21 Jul 2022 at 19:37...
Here's a making guide tyat answers most of your questions:
Once nitrogen dioxide forms, it is a waste gas; Nitric oxide bubbling indicates that the reaction is proceeding too quickly. Either the drip rate or the acid strength should be adjusted, you don't want nitric oxide (and its parents) boiling off as waste.
If using HCL, it's an equimolar reaction, and the pdf explains how to use a slight excess of the stoichiometry to guarantee that alcohol is the limiting reactant.
Do NOT stop the reaction when you see less blue nitrous forming and mope No2 gas evolving.
The saturation of an ester proceeds in a gaussian fashion, not a linear fashion. If you stop when blue nitrous evolution appears to stop, there are still several hundred thousand un-reactecd ions in the pot.
If you stop then, you might get 90% saturated of the alcohol (which sounds good in a linear process), but the difference between 90 and 100% saturation is profound.
The pdf ezplains how to determine for yourself, given YOUR reactant quality and preparation environment, when the reaction is complete.
You'll likely end up with ratios in the neighborhood of 1.00:1:10:1.10 moles of alcohol-HCL-NaNO2 or thereabouts
HomeBrewNovice said on Thu, 21 Jul 2022 at 21:34...
Thanks Professor....but is it still OK for the alcohol to sit on top while the nitric oxide percolates up through it? I'm assuming the nitric oxide is what's reacting with the alcohol to form nitrite? I'm assuming also that as long as I see tiny bubbles percolating upwards after addition, that the reaction is still happening as you suggest.
The Professor said on Thu, 21 Jul 2022 at 21:44...
There shouldn't be any NO bubbling; that indicates that reaction is proceeding too quickly and bloiling off reactants.
As written in the pdf i sent, the liquid phase prep is comprised of two steps.
In the first step, a strong acid (I recommend HCL at 37%) is introduced to the reaction vessel, which contains a top layer of alcohol, a bottom layer of sodium nitrite and water.
When HCL hits the NaNO2 (dropped under the surface to prevent exposure to the alcohol), H ions from the HCL bond with NO2 ions frtom the NaNO2 to form HNO2 ( a very weak acid that appears a royal blue).
That HNO2 proceed to float up into the alcohol and creates the alkyl nitrite (popper)
Nitric Oxide bubbling is NOT what you want
In a preferred environment (a very cold ice bath, around -12C, and a drip rate of approx. 1ml/min of 36% HCL that's been diluted to about 22%, it looks like absolutely NOTHING is happening.
This isn't brewing, some people tend to think that chemistry is just fancy cooking. The product is very fragile, and heat doesn't do anything favorable for you
HomeBrewNovice said on Thu, 21 Jul 2022 at 23:08...
Thanks again Professor for the explanation. So...bubbles and brown gas, both bad. But OK to see blue. I'll give this a go again to see if I can have better luck.
The Professor said on Fri, 22 Jul 2022 at 00:09...
Take your time, go slow and you shouldn't have much of an issue; after a few preps under your belt, it'll become familiar to the point of being boring. which I suppose is the point; reaction control is everything
TheMaster (Baiter) said on Fri, 22 Jul 2022 at 00:34...
PChef for the win on creating make believe wanna be nitrite cookers just to pimp his crap recipe that we all know produces the worst and nastiest stuff out there
HomeBrewNovice said on Fri, 22 Jul 2022 at 17:51...
@Professor.....I diluted my acid to about 20% hcl, which meant I ended up with more water overall. I went very slowly with addition, but the blue color kept getting darker like the alcohol wouldn't pick it up. At the end of addition, I increased my stirring rate and it helped, but I never broke surface with a vortex or anything. I let the pot sit until the bottom layer only had a few bubbles percolating up and the blue color was practically gone. Product seemed to have a very mild odor and good effects, but how can I get the blue acid to uptake to alcohol faster? Seems like it takes forever.
The Professor said on Fri, 22 Jul 2022 at 18:09...
The goal is to have the least amount of interaction possible with the equipment; that leads to mistakes.
Once you've created the nitrous, the second half of this two-step ion swap happens automatically; the nitrous floats up into the alcohol and satisfies it.
It's extremely difficult to get such a slow drip rate manually, and you've seen that going too fast wastes reactants to heat.
Alkyl nitrites are very fragile; the preps I do with the liquid batch process are 1 mol (about 120ml) and from start to finish takes about 3 hours.
If you want to do it faster, then you'll have to increase the HCL and NaNO2 molarity because you'll be boiling off and wasting those ingredients.
You'll also get more un-reacted alcohol, as the temperature will increase.
doing it right for human inhalation takes time, doing it quick and dirty will work for non-human purposes because acrid or poisonous by-products don't really matter in the 'legitimate' uses for alkyl nitrites.
I don't know if you read the pdf i posted, but it mentions that if the nitrous layer is constantly getting darker, it indicates that you are making nitrous acid faster than it is being consumed, and should slow the drip rate.
HomeBrewNovice said on Tue, 26 Jul 2022 at 00:38...
Based on what the Professor said about having no bubbles and a tame reaction pot, I have concluded that I was adding far too much acid and also too much sodium nitrite. It may be that if too much acid is added, the brew will end up weak. If a great excess of sodium nitrite is then added, there will be intense bubbling even if addition is done very slowly. This could taint the popper and give it less shelf life.
So....roughly equal molar amounts seems to be imperative - at least to prevent tons of bubbles and loss of nitrogen and perhaps give a better, longer lasting product.
The Professor said on Tue, 26 Jul 2022 at 20:40...
It sounds like you're getting a good ride; enjoy!
Unless otherwise noted, all contents of this website are
Copyright © 2011-2017 Jack Tinoco. That said, you can use my
images and article excerpts subject to these conditions.