Posted on Poppers Guide's Forum
Topic created by Charlie Chuckle
on Wed, 15 Sep 2021 at 19:35
Charlie Chuckle said on Wed, 15 Sep 2021 at 19:35...
I have been a visitor to this forum for many years, but never contributed because I haven't had anything to offer, but always incredibly grateful. I am no chemist, just an inquisitive guy who fondly remembers those sublime, nondescript, plain brown bottles purchased from behind the counter as a San Francisco guy in the late 90s - very early 2000s. I have opinions about then vs different eras but that's beside the point of this thread.
I have been culling this forum in my spare time trying to find the answer - going through years of posts trying to find the nuggets. Despite learning heaps from the contributions, I have not been able to find the answer here - nor other searching, so thanks in advance for indulging my 2 questions:
I've found that FCC NaNO2 can have 0.1% sodium mono and dimethyl naphthalenesulfonates added. I've done some reading about naphthalenesulfonates, and understand the intent behind including them, but can't find what it means for alkyl nitrites. What impact can naphthalenesulfonates have, if any, for practical purposes on nitrite synthesis during and after?
I have also read that there is a technique to simply separate oxidization/"impurities" of NaNO3 from otherwise ok NaNO2. But, this is where I have hit a dead-end for all practical purposes on how to refine crude NaNO2 fairly simply. I am incredibly grateful for any help because of my admittedly rudimentary skill set at this point.
The Professor said on Wed, 15 Sep 2021 at 20:24...
commonly described as anti-caking agent; safe and inert; it coats the granules of the powder so they don't clump when accumulating moisture.
Refining food grade and heavily oxidized NaNO2 isn't difficult; it just takes a heat source with low temperature swings at its set point.
NOT a stove (the thermostat cycling has a temperature delta that swamps the difference in melting points between niRITe and nitRATe.
Barely acceptable is a hot plate that can get up to temp; a heating mantle would be better.
The idea is to heat the powder (usually inside a ceramic crucible to help provide a more homogenous environment (temperature gradient between the surface and interior of the powder) to between the melting points of sodium nitRITe and nitRATe. The nitrite melts, leaving bits of solid nitrate, that are removed.
The remaining liquid nitrite can be re-crystalized, and will yield a sodium nitrite that is more pure and more dry than the best grade (USP) sodium nitrite, at fractions of the cost.
The Professor said on Wed, 15 Sep 2021 at 20:27...
The technique above works well for heavily oxidized nitrite; Sodium nitrite oxidizes slowly to nitrate; if you are using damp, clumped and discolored nitrite that has been laying around in an unsealed plastic bag for a year or more, it might be worthwhile to do the refinement.
If you are using dry powder, and the yield is still not right, it's not likely to be your NaNO2 that is the problem; it SLOWLY decomposes, and will last quite a long time if kept from oxygen.
The Professor said on Wed, 15 Sep 2021 at 21:09...
If the powder is not clumped, or only slightly clumped, and your product looks ill, you may have the stoichiometry wrong due to powder losses.
If the powder actually contains moisture, and you measure out 1 mol by weight, a percentage of that powder will be H2O, and when your react NaNO2 with HCL you want to get HNO2 and NaCL. The HNO2 goes on to nitrosate the alcohol, yielding the alkyl nitrite.
In this case, the contaminated NaNO2 will not completely react with the alcohol, and instead of nitRITe you get nitRATe, which has an un-pleasant aroma and effects .........not good or safe to inhale/
Charlie Chuckle said on Wed, 15 Sep 2021 at 21:30...
I was secretly praying that you would respond because you had partially answered my current questions in some of your past posts and I was digging more info. I cannot thank you enough for the detail. I had a hunch about the details you provided, but I constantly question myself whether I am chasing down the right path or if I am way off course because it's all purely theoretical in my head at this point, with no practical experience. I am the type that I want to at least try to do things right the first time, which can drive me a little crazy at times.
I will need some time to digest what you said and delve into how it would translate in practical terms for me (because as I said my skills are admittedly rudimentary at best at the moment, but I'm curious). I really appreciate your help and am humbled - and I hope that you will be so kind and patient again to indulge my questions in the future if I am questioning if I hit a dead-end on my end --- or whether I am headed in the right direction at least!
The Professor said on Wed, 15 Sep 2021 at 23:02...
no problem; I hope you get fantastic results