My home brew procedure

Topic created by MD_bottom
on Sat, 30 Oct 2021 at 17:14

MD_bottom said on Sat, 30 Oct 2021 at 17:14...

I made poppers at home for a number of years, with varying degrees of success, and then got away from it. I still have a 4L bottle of N-butanol as well as some n-amyl alcohol and concentrated H2SO4. I might want to order fresh sodium nitrite because what I have is years old. I think the alcohol shouldn't degrade, nor should the acid. The acid is stored in a glass bottle. But I think the sodium nitrite might at least have partially oxidized into sodium nitrate.

I used a process I found online.

https://www.designer-drug.com/pte/12.162.180.114/dcd/chemistry/eleusis/nitrites20.html

My procedure was to dissolve the sodium nitrite into distilled water in a beaker and then chill in the freezer while I prepare the acid/alcohol mixture. I then make a solution of 10mL distilled water, 13.9mL of H2SO4, and 55.1mL of Butanol. Chill that in the freezer. The put the nitrite solution in either an erhlenmeyer flask to a three-neck round bottom flask in a salt/ice bath. I then pour the acid/alcohol solution into a burrette, a little at a time, for dropping in the flask, using a flexible tube to make sure it is introduced below the surface.

Once the reaction is done, I transfer the contents to a large seperatory funnel and drain off the water and any sulfate that forms. I then wash the nitrite twice with a solution of sodium bicarbonate and salt to neutralize any leftover acid. I then drain off the nitrite into a small beaker and then add anhydrous sodium sulfate to absorb any water and transfer the finished product to an empty boston round bottle with a poly seal cap.

If anyone sees any problems with my procedure, please speak up. I'm not a chemist, so any info will be appreciated.

The Professor said on Sat, 30 Oct 2021 at 17:52...

That's about the gist of it. Using HCL rather than H2SO4 would be a cleaner prep (no precipitate from the sulfuric acid, no chance of scorching the alcohols (sulfuric is an extreme desiccant, it will burn you more severely than HCL if spilled, and will damage the alcohols if not introduced slowly.

Magnesium sulfate is a standard macro level drying agent, unfortunately it destroys nitrite. The nitrites are very slightly water miscible; a standard wash will leave mag sulfate dissolved in the yield, and destroy it from the inside.

If you're interested in the HCL liquid batch process, see our guide

http://poppersguide.com/forum/11682

Nitritespecialist said on Mon, 1 Nov 2021 at 17:32...

@MD....I started having better success by adding the SN solution to the acid/alcohol mixture. My brews were lasting far longer for example.

The Professor said on Mon, 1 Nov 2021 at 18:02...

@Md_bottom;
The weakest bond in a popper is the vine between the active ingredient (nitric oxide (NO)) and the alkoxy radical (the RO fragment).

That bond doesn't care ofotwasmade by dropping acid into nitrite, or by dropping nitrite into acid.

As mentioned in the guide, the preparation that drops nitrite into acid has a few downsides, one of them being that it generates much more acetate than the dropping acid method, since yield is constantly churning back into reactants.

TL;DR

Dropping nitrite into acid gives a sweet smelling product, and sweet smells indicate acetate rather than nitrite.

Acetate had no effects other than opposite; you might think that your product 'holds together ' longer, but that is not the case.

Sticking with the guide, and importantly, undergoing the preparation at very low temperatures, greatly reduces the possibility of noxious side reactions, and is capable of purity in the 95% or better range.

Nitritespecialist said on Mon, 1 Nov 2021 at 19:47...

@MD....if you are having some poor brews and if after trying all that the professor preaches you are still not having the success you had hoped for....you might want to try a different approach to how you mix. The German patent method from 2008 states to mix 40% SN solution to the acid/alcohol mixture because it has certain advantages. Also, the Professor himself mentioned an Italian study that described how they made their alkyl nitrites, by adding the SN solution to a mixture of alcohol/sulfuric acid. It's unclear why he hasn't criticized the Italian study's methods since it isn't even close to how he makes poppers. The Italian study, for example, uses 1 ml of 98% sulfuric acid per 1 ml of alcohol. That's a lot more acid than other literature has mentioned. Yet, they were testing their alkyl nitrites, via GC, immediately after making them and they were quite pure.

The Professor said on Mon, 1 Nov 2021 at 21:15...

what you are calling the "Italian" method of nitrite preparation is the preparation procedure that the chemists who wrote the publication used to synthesis a REFERENCE STANDARD from which to compare street samples to a known (and as pure as possible) sample.

A reference standard (like THE kilogram, THE inch, THE volt, THE second) is a curated sample of the absolute best possible accuracy, precision and repeatability.

The second, for example, is curated at the United States Naval observatory, and is extremely accurate.

"The observatory also operates four rubidium atomic fountain clocks, which have a stability reaching 7×10−16.

The clocks used for the USNO timescale are kept in 19 environmental chambers, whose temperatures are kept constant to within 0.1°C. The relative humidities are kept constant in all maser, and most cesiums enclosures, to within 1%. Time-scale management only uses the clocks in Washington, DC, and of those, preferentially uses the clocks that currently conform reliably to the time reports of the majority. It is the combined ‘vote’ of the ensemble that constitutes the otherwise-fictitious “Master Clock”. The time-scale computations on 7 June 2007 weighted 70 of the clocks into the standard."

A lot of time and money goes into maintaining a reference standard; it is a concept that exists above work-day level equipment. Nobody uses an Atomic clock to tell the time, for example, they use timepieces that have been compared against the atomic clock reference standard.

Taken in the context of preparing alkyl nitrites, a standard and an 'in-use' sample are two different things.

THAT's why the 'Italians' took so long to make 1 ml of poppers; because they were preparing a reference standard, not anything to be used for inhalation.

Nitritespecialist said on Mon, 1 Nov 2021 at 22:39...

Oh...OK...so nothing wrong with adding the SN solution to the acid/alcohol...it just makes a purer nitrite, good enough for a reference standard, and so also plenty good enough to be inhaled.

The Professor said on Mon, 1 Nov 2021 at 22:51...

The caveats are what kill your chances of success, EVERY time, for what, 12 yrs now?

If you want to take hours to make 1 ml of nitrite. ONE way to do it is in the dark, under nitrogen and with periodic shaking, while dropping nitrite.

The success these chemists had in generating a very nice reference standard doesn't translate to the prep YOU use; liquid dropping into a vigorously stirred reactor at nearly room temperature.

The prep as published is an anaerobic environment that isn't constantly churning reactants into the yield. Trying to adapt that method to a standard drop procedure COULD be succesful if undertaken at very low temperatures, and with limited stirring.

You didn't do that, you churned yield into oxygen and yield back into the reactants, which yields acetate and nitrate instead of nitrite, guaranteed.

The devil is in the details

Nitritespecialist said on Tue, 2 Nov 2021 at 16:12...

There ya go again...referring to shit that has nothing to do with the issue at hand, which is a variation, that YOU found on the web and shared, but then you elected to not speak of it because it didn't match up with your personally preferred methods. You side step that issue but tossing in irrelevant BS as usual.

I no longer make poppers as I've found a consistent reputable maker, Locker Room Marketing....they've been in business for over 20 years and don't resort to chatroom bullying, BS to sell their product.

The Professor said on Tue, 2 Nov 2021 at 16:56...

You just demonstrated willful ignorance; you know better, but it doesn't fit the agenda of your attack.

I explained why dropping nitrite into alcohol and acid failed for you (you introduced oxygen into reactants and mixed them together constantly, sabotaging your own prep.

That's not my fault, attacking me is not going to get you anywhere.

Now that you've personally decided to give up after 12 yrs, I don't understand the desire to sabotage others with the same incorrect ideas.

Nitritespecialist said on Thu, 4 Nov 2021 at 15:29...

Firstly, YOU have no idea what type of success I had or didn't have, because I never sent any samples to you. All you have is what I have stated repeatedly, that since I have a very high standard for popper quality, I wasn't satisfied enough with my own home brew - mostly due to variation and certain side effects associated with the butyls and isopropyl groups. But YOU did send two samples of your brews to me and well....we know how awful they were. So in the end, you have a very low bar for self reported satisfaction, whereas, I have a very high bar.

Nitritespecialist said on Thu, 4 Nov 2021 at 15:32...

So in the end it boils down to YOU being satisfied with toxic junk, which you falsely report to be some type of homemade elixir from heaven.

The Professor said on Thu, 4 Nov 2021 at 16:25...

this can't be who the name line says it is; another imposter?

A lousy imposter at that; i didn't send you two samples, that was a decade ago, and the results of that batch, while still in the infancy of my making, was well regarded by MOST of the people I sent to.

You ignore the fact that the sample I sent was prepped with a technique that YOU were proposing (well, not you, whoever you are, but ken jones).

You were suggesting a slight excess of the parent alcohol would somehow prevent degradation due to Le Chatelier's principle. THat idea, like any other idea ken has had, didn't pan out.

LIke anything that isn't Ken's idea, he threw a fit about how it 'smelled like the worst garbage he'd ever smelled.

Keep in mind that previously, he'd been talking about how his alkyl nitrite bought from a major chemical supplier had started to smell like rotten fish and vinegar.

Most makers here know what butanol smells like, and most can probably idealize what dead fish and vinegar smells like.

I propose that anybody who claims that butanol is more repulsive than dead fish and vinegar is Ken. (just kidding, but that idea smells fishy to me).

So, the takeback, for me, at that time anyway, was that Ken doesn't know what he's talking about (definitely, continuously) and that he will lie his ass off trying to debunk any work that isn't his.

Ken wonders why i keep bringing up the past. I do so because it informs people who didn't know him back then about what a lying, deceitful and dangerously un-knowledgeable pertson he really is.

Nitritespecialist said on Thu, 4 Nov 2021 at 17:12...

LOL....OMG such desperation. All I did was suggest a method of making nitrites from a web page you offered up on this forum. You recently stated the method mentioned was too time consuming, even though it did produce a 99.9% pure product, suitable for a reference standard. One would think a reputable chemistry Professor would want his adoring disciples to first make the purest compound possible so as to compare all other subsequent batches made using much faster methods.

The Professor said on Thu, 4 Nov 2021 at 18:31...

I'm not going to argue with whoever you are, but what you complain about sahows that you didn't understand what i said.

I DIDN'T say, for example, that a reference standard is suitable for use beyond the laboratory. Had you read my corollary to the atomic clock (which is actually a majority report of some 19 other clocks) you'd realize that reference standards are NOT to be used. Use often deteriorates them (the kilogram, for example, collects dust and changes its weight; if used in the field it would no longer be as accurate as it is under vacuum in a glass bell jar).

if a reference standard doesn't degrade by iuse, its cost is too much for field use.

It's laughable that I demonstrate exactly WHY a reference standard is NOT suitable for use, describe HOW the chemists succeeded in creating such a pure sample (it wasn't by dropping nitrite into acid. it was by undergoing the prep under nitrogen and with limited shaking of the reactions vessel), and explain how that's NOT the way to make product in bulk (it doesn't stay that pure for very long), and your response is "well if its good enough for a reference, then you're wrong about how to make" which is so ignorant, i can't imagine a more ignorant statement.

and we've heard SEVEDRAL ignorant statements from whoever you are

Nitritespecialist said on Fri, 5 Nov 2021 at 17:03...

The Italian method clearly stated they dropped the sodium nitrite solution into 1ml concentrated sulfuric acid(which you don't use) and 1 ml alcohol. They used this method for all the types of alkyl nitrites they made and tested.

Regarding reference standards, what disjointed garbage you manage to spit out!!!!

Nitritespecialist said on Fri, 5 Nov 2021 at 17:05...

And yes the chemists in the Italian study DID perform the synthesis under nitrogen, WHICH you NEVER do, nor do you advise to do.

The Professor said on Fri, 5 Nov 2021 at 17:07...

Are you trying to give Ken a bag name by speaking nonsense, or are you still trying to discredit me with stands in the dark?

I can't tell anymore