Super Fresh Pure-ish Food Nitrite

Topic created by MrFicken
on Tue, 12 Apr 2022 at 14:46

MrFicken said on Tue, 12 Apr 2022 at 14:46...

I managed to get my grubby hands on a sealed 50lb bag of food grade nitrite with a manufacturing date all of 2 months old.

Manufacturer by Chemtrade and came with analysis and all:

Sodium Nitrite >98.5%
Sodium Nitrate <0.8%
Water <0.3%
Disodium Carbonate <0.2%
Sodium mono- and dimethyl naphthalene sulfonate <0.2%

I was excited to try a batch and guess what the results were. Ficken horrible! Just as bad as the 2lb food grade from Duda. As soon as I spotted the bubbles that don't pop towards the end of the run I knew it was crap. Horrible horrible lethargy and nausea.

The COA for food grade %'s nitrite and nitrate is close or same as ACS grade which makes for lots of head scratching here. No way a sealed 50lb bag degraded in a couple of months.

Anonymous said on Tue, 12 Apr 2022 at 16:19...

@FuckedupBad....Try a boat load of sieves to suck up whatever mess you've created. The Professor claims it's a cure all. Of course, you may need a huge filter to get rid of all the dust/chunks the sieves will impart, lest you end up with a turbid cloudy bottle of shit.

Popperasswipe said on Tue, 12 Apr 2022 at 16:37...

The Professor says to test your alcohols....make sure yours didn't take a shit in the bottle. He says the old timers, the turn of the 20th Century chemists had discovered that the purity of the "alcohols" was essential. If you have a very pure alcohol, the right ratios or reagents....sufficiently cool temps....you will end up with a very high purity popper without any need to distill it.

The Professor said on Tue, 12 Apr 2022 at 16:54...

The professor says anonymous doesn't know what he's talking about haha the time, and the other half are blatant baiting lies.

sieves adsorb water, they don't fix anything toxic. Most soreness says made of clay like material that can make the liquid cloudy. There are sieves available that don't dust, but that doesn't matter to Ken because it's important to him that I be discredited, even say the expense of his own credibility.

The Professor said on Tue, 12 Apr 2022 at 17:00...

Popperasswipe:
I think you have the professor confused with nitritespecialist (Ken, now anonymous)

He's the one obsessed with last century musings that were later debunked. He's also the one that thinks alcohols degrade quickly, and had now become a teaching frantic junkie.

The Professor said on Tue, 12 Apr 2022 at 17:25...

MrFicken.

A bag doesn't prevent oxygen from penetrating. Still, two months from manufacture it should be valid (of, once you get things sorted it ends up being fine, please switch to glass bottles)

I'm not familiar with your prep, but you mentioned bubbles that won't pop.
You don't want bubbles at all.
Either the larger bubbles, or the pin and needle size bubbles. The reaction is at too high a temperature and is likely to be producing side reactions (a handful of side reactions can cause lethargy/nausea).

I suggest that it's likely not the reactants, but rather the prep method.

Even if you have had prior success with your method, please try going lower in temperature and developing a consistent method for flow rate.

At -12C ice bath, and a very slow drop rate, under the surface so as not to be involving oxygen as much as possible.

I've posted flow rates before ) of the trip of my head, something like 1ml per min for the first half hour, then about 1.5ml/min)

I don't suggest drying with mag sulfate.

Despite Kens rantngs, we have JUST under a hundred makers in our group that disagree with his insanity, and he'll pull his own teeth out trying to prove us wrong, but we have been having great success for the 12 years he's been failing.

Again, search for particulars (or join the Poppermakers group on Reddit) here.

It's something like a 2qt mixing bowl with 350g of salt (not iodized) and the remainder ice that has been crushed into snow.

At such a low temperature, and removed from air, there isn't enough energy on the reaction vessel to allow side reactions, the entire reaction is without drama, no swirling, no bubbles, and no wasted acid from boiling off reactants at such high temps.

Good starting ratios are 1.00:1.02:1.05 mol alcohol to NaNO2 to HCL

The reaction should be boring, no bubbles or swirling, and the results should be much more repeatable since you're no longer trying to pick up a sand dollar in the tumbling surf)

MrFicken said on Tue, 12 Apr 2022 at 18:22...

Just setup a reddit account to join that group mentioned above. I do appreciate all the feedback. Well almost all of it. Sieves ain't gonna help issues with using food grade. Also all my alcohols are fresh and ACS grade. Shelf life for alcohols and HCl aren't much of a concern anyways. I have no issues using ACS grade nitrite. Results are always perfect when I do. Only challenge is finding the perfect mix of alcohols for the effects I am interested in at the moment. I have managed to create some really novel stuff (outside of amyl, butyl, & the propyl). No issues controlling a reaction and understanding the stoichiometry required.

My only challenge is using food grade. I have tried a few approaches at refining food grade assuming it was age degraded. Seems that isn't the root cause given my two month old 50lb bag was crap. Refining was better but not even close to ACS. I took samples from top middle bottom and all of the products from the 3 runs were complete crap. Only change was the nitrite food grade vs ACS. I have ordered some ACS nitrAte and will do some runs mixing it in increasing ratios to ACS nitrIte (can't wait to work out the stoch for it arghhh), and then 'sampling' the product. Thinking here is do a few grains of nitrAte tmake crap product or do you need loads. If so how much? Also, it is nitrAte in the food grade nitrite the cause?

The Professor said on Tue, 12 Apr 2022 at 19:06...

Sounds like you have a solid foothold on what you are doing. IME, the only time i've had trouble with NaNO2 (even when i was buying food grade from duda diesel) was before they started using anti-caking agent.

Their lot numbers were always about 3yrs old, and if stored casually they'd clump (changing the weight from atmospheric water absorption) and degrade to NaNO3 (which can lead to nasty side effects), and eventually become discolored and choked with naNO3. Personally, once I 'made up' for the loss by increasing the powder to the point of 1.2 mol (a 20% excess), the results were horrible.

I wasn't interested in many of the NaNO3 reduction procedures because i didn't want to work with lead, and why would i need to convert nano3 to nano2, wasn't it better to somehow filter the smaller amounts of degraded NaNO3 out of the NaNo2 I already had?

So I started refining it through separation of melting points. It's a bit fiddly with a mantle and crucibles required (unregulated stovetop WILL liberate O2, but is guaranteed to also be above the decomp temp of NaNO2).

TL;DR I ended up with the purest, driest NaNO2 available from food grade.

Duda has started using an anti-caking agent. Their lot numbers are same year (at least for now) and the product is very suitable for the prep.

Looking forward to hearing from you!

Anonymous said on Tue, 12 Apr 2022 at 20:31...

I have included two Youtube videos that clearly show that to make IPN, one should use a molar ratio of HCl that is about 1.3 to 1.45, as the Professor so dutifully figured out. Also, temps as low as -12C for IPN will absolutely yield very little.
There is nothing wrong with food grade SN, provided sufficient acid is used and the alcohols are not degraded.

Bubbles are fine...they indicate a reaction is taking place. I had big bubbles when making IPN, and right near the end of addition, everything becomes tame, indicating that enough reactants have been added and the reaction is nearing completion. It would take forever to make IPN if you added one drop per minute. It's not necessary.

Anonymous said on Tue, 12 Apr 2022 at 20:33...

The Professor has no clue what my home brew poppers are like...except by what I have stated online.

On the other, I have tested his samples and can vouch that they were cloudy, turbid toxic shit that smelled far worse than anything I botched.

Anonymous said on Tue, 12 Apr 2022 at 20:46...

And mind you, this was ten years ago, when he was claiming his poppers were perfect.....

kens-anus said on Tue, 12 Apr 2022 at 20:46...

ken can go back to his corner. The original poster knows fact from fiction. That side reactions require energy; that colder is better; that alcohols don't age very quickly; that HCL is very stable.

Quick question genius; since HCL and NaNO2 are BOTH required to produce HNO2 (HNIO2 being the mild acid that actually satisfies th alcohol), and you are thinking that an excess of HCL will somehow force the reaction to completion, my question would be HOW can HCL nitrosate ANY alcohol without NaNO2.?

IF your idea was doing ANYTHING other than boiling off most of the excess and making table salt with the rest, the alcohol would require an excess of HNO2, NOT just HCL, and you don't get to HNO2 from HCL without NaNO2. the 'large excess of acid prep at near room temp' idea discredits itself.

Anonymous said on Tue, 12 Apr 2022 at 20:54...

And the reason I KNOW a greater molar ratio of HCl is necessary is because I was using the ratios the Professor just mentioned....and 100% of the time, I got toxic IPN and N-butyl ntrite.

Now, after watching and reading what others have done....seeing the Molar increase in HCl.....and putting it into practice....I have seen what a HUGE difference it makes. You need to push the reaction to the right....and you won't be able to if you don't add enough acid.

kens-anus said on Tue, 12 Apr 2022 at 20:56...

readers; quick question.

why is it that ken repeats the same BS as if we haven't heard it thousands of times over?

When he says 'the professor's poppers were cloudy and toxic' do you think he's revealing some hidden secrets that i'm trying to avoid, or do you understand that he is trying to manipulate opinion through lying ?

remember that cloudiness was from dusted sieves (that adsorb water)? Do you remember that it makes no difference to the VAPOR if the liquid is transparent?

When he repeatedly claims that popchef's 98% pure n-Butyl nitrite with 10% unreacted alcohol (street samples of OTC poppers often contain 40% unreacted alcohol (by way of comparison) was nasty and toxic?

or do you realize that he's magnifying any trifle he can think of to convince people that i'm a charlatan?

I am truly curious at this point

kens-anus said on Tue, 12 Apr 2022 at 21:13...

careful Ken; people may start to think you do this on purpose; offering insane prep ideas, so that I can follow up with actionable information that yields results.

If that's the scene, then i guess it's a wild success.

Years ago, you pointed an interested person on reditt toward popchef. That's where I became familiar with him; just after the guy that was observing the discourse between yourself and popchef decided that you were ignorant of required information and that popchef was suitable.

WE worked on a simultaneous preparation and distillation process together. I bought a new audi R8 with the proceeds. lots of fun!

When you abandoned poppersplace, many of the members that you had abandoned got together with popchef and started their making group, and we've been very happy and satisfied with the results of a liquid batch prep at -12C. we DO get yield (we know there's a protracted reaction vessel residence time) because we know what we're doing.

In the months that either myself you popchef have been posting here (an accident actually,) you have personally pushed a handful of makers our way (again, not on purpose, but by comparing the lies you spout with the information i provide) and their world is a better place without your BS.

The whole deal sort of validates itself. Keep ken AWAY from the grownups table (so he doesn't rant lies and ignorant ideas, wasting people's time) and his nonsense will drive those scientifically inclined to understand reality to seek out the truth, which is as far away from ken as possible

Anonymous said on Tue, 12 Apr 2022 at 22:46...

Those "chemists" who took the time to post IPN making videos would be the perfect people to ask why they used quite a molar excess of HCl.

When you do it and it works.....over and over again....you no longer question the wisdom of it.

kens-anus said on Tue, 12 Apr 2022 at 22:56...

And a nod's as good as a wink to a blind man. Thanks for being you

Rodney King said on Wed, 13 Apr 2022 at 03:51...

Damn there is a lot of drama in here! Can't we all just get along?? The smaller your batch the more room for error. Try doing batches that take 20# of SN! That would be two pails from DUDA. Maybe that is a little too much product for you....but seriously.... Once you collect your liquid gold, no matter how it looks, try adding some baking soda and some table salt and maybe a little H2O. Do not worry about having a little water/trash in the bottom. Stir and then add some MS anhydrous. Stir it up, let it settle, and all the trash will be consolidated in the bottom. water/trash in the bottom will be absorbed. Pour off the good stuff. The rest will remain behind like sand/gravel. The yield is usually a little more than the volume of the alcohol you used. On a side note, maybe try adding crushed ice to the mix instead of the ice/salt bath. Water in the mix is irrelevant in the end and may even help pull out the trash. One more note, a lot of you are using way too much acid from what I have seen here and on reddit....thus the nasty and spooky and DANGEROUS smoke. If you get a profound reaction to the baking soda during washing that proves you used too much acid. Store your clean and pure liquid gold over 2-3% by weight potassium carbonate to keep it fresh and stable.

Anonymous said on Sun, 17 Apr 2022 at 18:04...

The problem with using 20 lbs of SN all out once is that what if the product is garbage...or won't last? You just wasted a whole lot of shit. There is absolutely no guarantee that the product will last more than a few days.

I just used new 2 lbs Duda SN and got a somewhat improved amyl nitrite. But I also used excess acid.

Product has a somewhat spicey, medicinal scent...mild, but akin to menthol NOT camphor. Effects are OK....nothing weird or over the top.