46% Yield - What is yours?

Topic created by WaPopperBator
on Fri, 16 May 2025 at 18:53

WaPopperBator said on Fri, 16 May 2025 at 18:53...

I'm going on my 3rd batch of quality poppers with a 46% yield. That is to say, if I start with reagents for a 500mL batch, I'm ending with 230mL of poppers.
How is this in comparison to the old pros and experts?

The Professor said on Fri, 16 May 2025 at 22:18...

I had to check my notes, and it depends on if you mean raw yield ( measuring before neutralizing (neutralizing destroys some yield, but prevents acidic results)

raw yield I typically get 103% (this includes unreacted alcohol and acid).

final yield is typically 98.4% (the final neutralized, preserved and stabilized product)

Poon said on Sat, 17 May 2025 at 00:00...

Hello The Professor. I believe you have calculated theoretical yields for these reactions. Roughly what conversion is expected?

Poon said on Sat, 17 May 2025 at 00:03...

Also, The Professor, is your synthesis guide still available? Thank you.

WaPopperBator said on Sat, 17 May 2025 at 01:22...

Wait....after stabilization and balancing pH you're getting 98.4%? What batch volumes are you typically doing?
Impressive. I have much to learn.

The Professor said on Sat, 17 May 2025 at 17:47...

@Poon:
Of you want theoretical towels, the equation is equimolar; no calculations needed.

The results o posted are percent of theoretical, iow actual.

@WaPopperBator:
I no longer run a batch process, but rather a hybrid continuous process.

The Professor said on Sat, 17 May 2025 at 17:48...

Towels should be yields

The Professor said on Sat, 17 May 2025 at 17:50...

Towels should be yields

Poon said on Sat, 17 May 2025 at 18:26...

The Professor: Above you indicated that some of the alcohol goes unreacted. Did you not previously post some thermodynamic results?

Poon said on Sat, 17 May 2025 at 18:39...

Also, would you please repost your synthesis guide?

The Professor said on Sat, 17 May 2025 at 19:08...

@Poon;
i was quite active here years ago, I probably did

Dr. Wang said on Sun, 18 May 2025 at 02:29...

I've never measured yield, I'd only bother if I were distilling. It's about the same volume out as in. What The Professor said.

Dr. Wang said on Sun, 18 May 2025 at 03:08...

The Professor's like "I'd better field this one before that wang retard chimes in... the David Spade of Chemistry"

A continuous process, you say? Are you manufacturing commercially?

The Professor said on Sun, 18 May 2025 at 17:14...

@DR. Wang;
If you don't measure yield, you'll never know how incremental changes in variables effect the conversion efficiency and purity.

e.g. At first, I was happy with 95% yield, until further runs revealed that my 95% yield still had about 10% unreacted alcohol dissolved into it.

I'm a retired chemical and electrical engineer; this stuff is fun for me. I don't manufacture commercially. I started with a batch process and a dozen 'volunteers' to help me tune the apparatus. That population has grown considerably, and batch processing would take too much time. It also was a fun challenge to switch to a hybrid continuous process.

I don't sell online.

I'm just answering a question posed by the OP, I have no other agenda.

mr impossible said on Mon, 19 May 2025 at 19:41...

110 % expected idk how. my math must be off or its cause i added a step that i dont think others do.

duh said on Mon, 19 May 2025 at 19:44...

its because calculated yield using the little bottles themselves and not actually measuring the whole yield itself.

The Professor said on Mon, 19 May 2025 at 20:55...

CALCULATING RAW YIELD:

the balanced equation is equimolar; one mole of each reactant in, one mole of product out.

This is the theoretical yield.

In this reaction, the alcohol is the limiting reactant, meaning that, theoretically, an overabundance of any of the other reactants won't create more product.

Thus, you can reduce the math to one mole of alcohol in equals one mole of product out. (it is an alcohol nitrosation after all).

Since the reactants and product are of differing densities, one can't simply measure ml; converting to molar quantities will take density differences into account.

If moles of product exceeds moles of alcohol input (>100% yield), and depending on reaction temperature, this would indicate that either the apparatus was loaded with an excess of acid, or the product is tainted with unreacted alcohol, or both

General guidance for this type of reaction calls for a slight excess of acid and powder, again, depending on temperature

Dr. Wang said on Tue, 20 May 2025 at 03:19...

>I have no other agenda
I never meant to imply sir, I'm just impressed and curious, I meant no offense. Your reputation precedes you.
I've prepared several batches using both slight and significant excesses of the nitrite salt and acid, but observed no discernible differences myself- I’ve also conducted reactions with as little as 60% of the stoichiometric requirement for HONO, again without any noticeable difference. However, I have not been quantitatively measuring yield or density, primarily due to the small scale of the batches. My issue has always been shelf life. I've always been satisfied with my own product, but I still have a lot of unanswered questions and kinks to work out.

The Professor said on Tue, 20 May 2025 at 21:35...

@Dr. Wang,

I'm probably a bit gun shy on this forum, as previously I've been dragged through the mud and accused of nasty things.

Nitritespecialist said on Tue, 20 May 2025 at 23:28...

@The Professor

How DARE you accuse me of accusing YOU of things. If anyone was dragged through the mud, it was ME. I perfected a recipe for amyl nitrite which you hobnobed for years. SN purity is THE absolute biggest thing to getting the reactions right followed by purity of alcohol. You suggest to use HCL and I use Sulphuric acid which works better because it does not act as a nitrosating agent. Any time I brought up THE FACTS I was hobnobed by you trying to spread disinformation and get people killed.

Poon said on Tue, 20 May 2025 at 23:44...

The Professor: For the third and last time, is your maker’s guide still available?

The Professor said on Wed, 21 May 2025 at 19:04...

@Poon,
If you are new to this forum, and don't understand that it has a lingering infestation of dipshit stupid, then you are probably frustrated by my lack of response.

It's not worth my time, or yours, to try to get words of truth in, edgewise, against the torrent of ad hominem attacks and potentially lethal advice we'd both be bombarded with, from such a purposefully ignorant creature as above.

If you aren't new, you know what I mean; if you are new, all of his drool has been archived in prior posts; this guy has been pretending to be a poster from more than a decade ago, who since has gone on to who knows what; although that guy (Ken) was himself inept, this version of him (specialist, expert, mo'ass, and various alias) is, something else entirely.

If you are truly interested in what the inside of his rectum sounds like, google

site:https://poppersguide.com/forum/: The Professor

you'll see how uninformed and downright dangerous some of his ideas are, how nasty he is, and how he contradicts himself just to waste reader's time.

That said, if you have specific questions, and can tolerate the post thread being infested with BS, just post your question, and I'll answer to my ability.

Dr. Wang said on Thu, 22 May 2025 at 11:38...

(Sorry MAM, this one's cleaned up a bit better)

Gee, I'm probably going to step into a hornets nest here, but it looks like before the continuous process, The Professor based his method on Vogel's. It involves fully dissolving the salt and introducing the acid/alcohol mixture through a funnel at the bottom of the vessel? I'm honestly not sure what value there is in doing this and observing the color change, but I haven't tried it, and I'm not an expert, so I'm not going to knock it without trying it a few times and really understanding it. I've had entire batches remain blue with persistent nitrous acid, and I've had the color dissipate on warming to room temp or washing. In the end, I've had killer product with a runaway reaction that heated up and billowed brown fumes. My issue is stability.

The involved parties are free to correct me. I'm not here to argue, I'm here to refine my product and assist where possible. I have lots of reading ahead.

Hey- PoppersGuide.com rated a couple citations by ChatGPT!

---

### Vogel’s 1974 Procedure for Synthesizing Amyl Nitrite

*Materials:**
95 g (1.38 mol) of sodium nitrite
375 mL of water
25 mL of water
62.5 g (34 mL) of concentrated sulfuric acid
110 g (135 mL, 1.25 mol) of n-amyl alcohol (pentan-1-ol)
Ice-salt bath for cooling
Mechanical stirrer
Separatory funnel with stem extending to the bottom of the flask
Thermometer([2], [3], [4], [5])
*Apparatus Setup:**

Use a 1-liter three-necked flask equipped with :-( [5])

A mechanical stirrer
A separatory funnel with a stem extending to the bottom of the flask
A thermometer([5])
*Procedure:**

1. **Preparation of Sodium Nitrite Solution:**

Place the flask in an ice-salt bath to cool it to 0 °C.
Dissolve 95 g of sodium nitrite in 375 mL of water within the flask.([4], [2])

2. **Preparation of Acid-Alcohol Mixture:**

In a separate container, mix 25 mL of water with 62.5 g of concentrated sulfuric acid.
Add 110 g of n-amyl alcohol to this mixture.
Cool this mixture to 0 °C.([4], [3])

3. **Addition of Acid-Alcohol Mixture to Sodium Nitrite Solution:**

Slowly add the cooled acid-alcohol mixture to the sodium nitrite solution in the flask over 45–60 minutes.
Maintain the reaction temperature at approximately 0C (±1C) throughout the addition.
Ensure vigorous stirring during the addition to promote efficient mixing.([4], [2])

4. **Post-Addition Stirring:**

After the complete addition of the acid-alcohol mixture, continue stirring the reaction mixture for an additional 1.5 hours while maintaining the temperature at 0C.

5. **Separation and Purification:**

Allow the mixture to stand, then filter off the precipitated sodium sulfate.
Separate the upper yellow layer of amyl nitrite.
Wash this layer with a solution containing 1 g of sodium bicarbonate and 12.5 g of sodium chloride dissolved in 50 mL of water.
Dry the washed amyl nitrite over anhydrous magnesium sulfate.([3], [6])

6. **Yield and Distillation:**

The crude amyl nitrite obtained should weigh approximately 107 g, corresponding to a 73% yield.
Distill the product; it should distill at 104C with negligible decomposition.
Under reduced pressure (40 mmHg), the boiling point is approximately 29C.([4], [5])
*Safety Note:**

Amyl nitrite and other alkyl nitrites are volatile and can decompose upon standing. They should be stored in a cool place and used within a few days to two weeks of preparation. Decomposition products can include water, oxides of nitrogen, the parent alcohol, and polymerization products of the corresponding aldehyde.([3])

---

[1]: https://www.scribd.com/doc/46458376/Vogel-Practical-Organic-Chemistry
[2]: https://vdoc.pub/documents/vogels-textbook-of-practical-organic-chemistry-6effnvua2rb0
[3]: https://poppersguide.com/forum/12195
[4]: https://vdoc.pub/documents/vogels-textbook-of-practical-organic-chemistry-509l3k4igkh0
[5]: https://poppersguide.com/forum/12450

The Professor said on Thu, 22 May 2025 at 15:45...

@Dr Wang,

Back when I was just starting, I tried Vogel's. The first 10 runs of that gave me enough data points to start tweaking my own prep.

Dropping underneath the yield layer is crucial, it prevents HNO2 from being exposed to air, and turning into nitric acid.

It also prevents constantly dropping high strength acid into the yield layer that developes on the surface, which hurts yield

I find HCL superior to H2SO4, especially at low temps. Sulfuric requires a much slower drop rate to prevent desiccation of the alcohol, and the paste like condensate frustrates magnetic stir bars.

All this intermediate stage needs is hydrogen, and it's much easier to deal with chlorides than sulfides.

Also, I no longer drop acidified alcohol into sodium nitrite solution; when using the batch process I get better results dripping sodium nitrite solution into acidified acid (HCL, this would likely 'scorch' the alcohol if one uses sulfuric )

I didn't bother to check the stoichiometry; videos prep is at 0C, which still had way too much latent energy floating around, and proper stoichiometry depends very much on prep temperature.

Excess energy is asking for unintended side reactions.

The Volgel prep is intended, as are most published preps, as an in situ prep for small amounts and immediate use, often for diazotization reactions, and doesn't address stability

For stability, first you need a much more pure yield, as the most common side reactions speed up decomposition.

Have you tried potassium carbonate to slow decomposition?

Dr. Wang said on Sat, 24 May 2025 at 03:18...

Thanks for all the information Professor.
You know, I've tried just about every drying agent *except* K2CO3.

>"this would likely 'scorch' the alcohol"
Do you suppose this might also be a danger if using gaseous HCL or nitrosylsulfuric acid? NurdRage did a recent video using the latter.

>"Excess energy is asking for unintended side reactions"
I tried dry ice a couple of times, but it seemed to stall the reaction so much that by the time all the acid was added, nothing appeared to happen, and I had to very slowly and carefully raise the temperature of the mixture to get the reaction going but prevent a runaway.

How much emphasis do you place on excluding air? I sometimes use air duster as a blanket (difluoroethane/152a). It's extremely water soluble, as are the bitterants. Any idea if this would be compatible in this case?

The Professor said on Sat, 24 May 2025 at 18:58...

@Dr. Wang,

On drying agents; of the common driers, simple calcium chloride does the job as well as any other, and doesn't promote degradation like Magnesium sulfate will.

None of these quick driers are sufficient, they remove water better than the gross separation of waste layer from yield through separation funnel though. IMO the drying step isn't very critical, since I store the yield over MS3, which removes water down to a few PPM after 4 days.

K2CO3 is used in those glass ampoules that started the whole poppers thing. It slows degradation by preventing NO gas buildup inside the ampoules. IIRC, about 1% w/v does the trick. Excess will have negative effects.

Re scorching: the general guidance re acids is that sulfuric is preferred by industrial processes because it is cheaper, and HCL is preferred by chemists interested in a clean source of H ions. Sulfuric is much more dessicating than hydrochloric, a drop on your finger will demonstrate this, sulfuric will burn and HCL won't.

Gas phase preps work too, but are more dangerous for the layman.

AFAIK, nitrosylsulfuric is a solid until 150f or so; maybe it was ground into a powder and dissolved in sulfuric? regardless, we only want the H ions, and don't like dealing with the sulfates.

Dry ice: by itself will likely solidify the batch, or at least turn it into a paste-like slurry. We have a maker who swears by it, but he uses an ice bath regulated to -15C instead of raw dry ice. It's simple to get down to -15C or so with only salt and crushed ice; if you want less mess, chemical baths can be used, but the waste is more toxic, and should be disposed of as hazardous.

Excluding air: the product is sensitive to hydrolysis, pyrolysis and oxidation. A layman would think that it's preferable to eliminate any sources of light, heat and O2 during prep.

It DOES make a very small difference during prep, but the two step batch process requires water as a solvent; removing water during prep (e.g. using sulfuric acid or a lower amount of water prepping the NaNO2 solution, is starving the reaction.

Blanketing the apparatus or using a vacuum manifold isn't worth the trouble; for the amount of time the yield is exposed to O2, not very many molecules will be interacting with the air (that is assuming that your magnetic stir bar is set at a very slow speed, NOT creating a vortex of fluid that is constantly churning O2 into the yield). I DO cover the reaction vessel with cling wrap.

WaPopperBator said on Sat, 24 May 2025 at 21:16...

Thank you to everybody who contributed to this thread! You're really helping me make my production procedures improve. When my leather cleaner hits the market, I'll let you know!

Scott McCusker said on Sat, 24 May 2025 at 23:43...

That is scrotally awesome!

Scott McCucker Carlson said on Sun, 25 May 2025 at 22:11...

> Dropping underneath the yield layer is crucial, it prevents HNO2 from being exposed to air, and turning into nitric acid.

Dipshit. The top layer is the alleged ester if you did your rxn "correctly." HNO2 is in aqueous solution BELOW that. You would know from your own procedure that you keep these things stratified because you call for NO VORTEX, just enough to break surface tension. That's a good call, but apparently, you don't remember ever saying it.

You mix BELOW the top layer as to not destroy it with protons. Funny thing is that depending on your rxn parameters, the top layer is still undergoing the rxn (excess NO? Maybe, maybe not), so it makes good sense to shield everything with an inert gas like N2 or Ar. I prefer Ar because it's not going to go wandering off.

"Professor" was paid about five years ago to keep his mouth shut. We were guessing whether he had some Dean-Stark apparatus or was doing a flow reaction, and he's senile enough now to tell us that it's the latter.

The Professor said on Sun, 25 May 2025 at 23:17...

5 years ago? I had moved from batch phase to gas phase prep, mostly because I enjoy chemistry, If I got paid to keep my mouth shut, then I demand payment!

I didn't use a dean-stark apparatus in the batch phase.

I just recently switched to a continuous flow prep, so the 'we' that were guessing had no idea what I was up to apparently, and now want to attack me because they are taking things out of proper chronology

I did mention that a vortex in the rx chamber is not good, AND if you drop to the surface, you'll destroy yield AND create clouds of NO2 from HNO2 reflux to the surface (when the acid hits the NANO2 to create HNO2, some will get spit up onto the surface and create an NO2 cloud)

Kind of like how when the shit hits the water, that drop of water shoots up your ass.

The NO2 generation diminishes as the surface builds up yield, but it DOES happen, and can be visibly confirmed;

I've run preps with vacuum manifolds, and with Ar blankets; simply covering the Rx vessel with cling wrap and a slow stir speed is sufficient; for the amount of time the surface molecules are being exposed to air, it's not worth the extra expense.

I (don't recall stating that the top layer is still undergoing reaction; maybe at first, but as the yield is created, it floats to the surface. If you look down into the Rx vessel, you can see the reaction taking place UNDER the surface.

As a senile dipshit, i find your entire post to be full of ad hominem attack, misunderstood straw man fallacy and outright incorrect assumptions.

These guys and gals don't care about my mental status (or yours); they just want to make something nice and strong and smooth..

TopOfThePops said on Wed, 28 May 2025 at 23:52...

@The Professor is a good Dude, if this is who it sounds like (aka Pop Chef). I used to be part of a group of DIY brewers who followed on Reddit. I tried his Recipe, including dropping beneath the upper layer (yield) to prevent scorching and all the SOP exactly. I am not a Chemist, zero chemistry background. Just a guy who stumbled upon Pop Chef (The Professor) and he was always a Gentleman, even going so far as to include me as his test party to those early batches, never charged a dime! Unfortunately, I lost contact and was never able to replicate a DIY batch which approximated those store bought brands I remembered from the 1980's and 90's. I do not think I have/will come close to anything as good and pure as those products. So, after a few years of DIY attempts and many hundreds of dollars for Supplies I threw in the towel. Now if The Professor would be willing to allow me to partake in his current vintage, I would be very grateful! Not sure how to establish a contact outside of this Forum thread? Anyway, what I learned was the SN is hard to source (pharmacy grade that is, not food grade). Otherwise, as I said I followed the Pop Chef SOP exactly, very strict adherence but never quite got 'there'. Ice bath temps, very critical, drip rate extremely important, exact ingredient math and measurements critical, and following safety protocols with where to brew and limiting exposure during processing with breathing apparatus being worn, etc... Basically, there is no room for mistakes and ultimately it comes down to quality ingredients used and strict adherence to SOP and keeping a detailed log for fine tuning. Good luck ya'll

Md_bottom said on Thu, 5 Jun 2025 at 23:59...

With sodium nitrite becoming hard to get because of that guy selling his suicide kit, I'm wondering if switching to potassium nitrite is an option. It should work just same.