Posted on Poppers Guide's Forum
Topic created by Charlie
on Sat, 4 Dec 2021 at 09:03
Charlie said on Sat, 4 Dec 2021 at 09:03...
For this attempt, I decided to do a half-mol of butyl. I used a 28 mm OD, 25 mm ID glass tube fitted with a #4 rubber stopper with one 5-mm hole for the dropping tube. The 5-mm hole fit the the 3/16" OD chemical tube from the peristaltic pump well.
Again this time, the reaction vessel (600 mL tall form beaker) was frozen into a 64 oz. Pyrex measuring cup. This sat on top of a magnetic stirrer fitted with a temperature probe holder inside of a chest freezer set to -6F. I replaced the probe holder with a burette clamp to hold the dropping tube, which sat just below the water line. The peristaltic pump sat outside the freezer and tubes ran through the drain hole. The acid sat in a boiling flask on top of a cork flask holder inside of the freezer. I lightly covered the reaction vessel with plastic wrap.
I dropped the 55.5 mL acid water mix over 101 minutes. This equals about 3 hours 22 minutes for a full-mol reaction. I actually mixed 50 mL 37% HCl & 11 mL distilled water so that there was enough overage to prime the pump, which takes about 5 mL.
-The contents of the reaction vessel started out at -17.5C
-After 15 minutes, it was -19.2C
-After 30 minutes, it was -18.8C
-After 45 minutes, it was -17.1C
-After 60 minutes, it was -16.6C
-After 75 minutes, it was -16.4C
-After 90 minutes, it was -15.7C
-At 101 minutes, it was -14.8C
When I checked it at 75 minutes, the waste phase was a pale blue. However, white, opaque crystal-like structures had formed around the outside of the dropping tube in the yield layer, with some on the surface of the yield as well. Before this point, the solutions(s) were pale yellow with no crystals. I raised the dropping tube very slightly at 90 minutes and the crystal-like structures seemed to get mixed back into the solution(s) and disappeared for a few moments, but then they reformed in the last few minutes.
This mimicked what I saw last round, but more extreme. They seemed to completely disappear once I moved the solution(s) to continue agitating for 15 minutes once all the acid had been dropped. I am wondering what these structures were, why they appeared and what they mean. Was the final yield layer getting too cold - or was something in the yield layer freezing? I didn't notice them the first two attempts which were done under warmer conditions. This was the coldest attempt yet and these structures were worse than last time, which was also warmer by a couple degrees Celsius.
Raw yield was just over 50 mL and the final yield after neutralization was 41 mL. It is currently drying on molecular sieves.
Nitritespecialist said on Sat, 4 Dec 2021 at 13:56...
@Charlie...I don't know.....perhaps pyridine crytals? This was found to be an impurity in some alkyl nitrites. If present, they can be washed away with water. Otherwise, pyridine is toxic to inhale.
Charlie said on Sat, 4 Dec 2021 at 17:03...
TY Nitrite for the tip.
I'm going to try again shortly staying a few degrees warmer and see if I have the same thing happen. Whatever is happening seems to get mixed back into the solution(s) with a little more agitation or increase in temp. I'm wondering if starting out at -19C and ending up at -15C is just too cold...
The Professor said on Sat, 4 Dec 2021 at 20:16...
Pyridine is not an impurity, it is a stabilizer, and would have to be included in the prep to be present in the yield. Unless you purposefully included pyridine to stabilize (I do'nt recommend that, it smells like dead fish).
It is used as a stabilizer for alkyl nitrite in some of the large chem manufactrurer Alkyl nitrite, which aren't intended for inhalation.
What you were seeing is very likely the yield starting to freeze over
The Professor said on Sat, 4 Dec 2021 at 20:22...
water soluble impurities cannot be 'washed away' with water, as suggested above. Washing is technically a liquid - liquid extraction. If you want to extract a water soluble, you must use water AND an ingredient to ATTRACT the impurity of concern.
e.g. a liquid-liquid extraction with brine (salty water) removes the impurity H2O because salt is attracting water molecules.
If you want to extract pyridine from alkyl nitrite, you'd have to use an ingredient that attracts pyridine in a water solution, NOT just the water itself.
Charlie said on Sat, 4 Dec 2021 at 21:49...
I think you're probably right because this prep was colder than the last and the crystals were more abundant. They all but disappeared when I turned up the stirrer a little and left the freezer open a little thereby increasing the ambient air temperature. I noticed the solution temperature is not completely consistent if the stirrer is agitating at a very low speed so it could be that the crystals unfreeze once I turned up the stirrer to homogenize the solution(s) temp. Just my theories ATM. Will try to shoot for consistent -12C next time and report back but it seems the yield is freezing. If so, do you know of effects good or bad?
Prof., I also noticed something else that piqued my interest. This attempt, I first chilled the alcohol separate from the NaNO2 + water. I chilled them to -18C, then mixed them. Immediately, the temperature spiked to -8C. I then rechilled the alcohol + NaNO2 + water down again to start. Does this temperature spike indicate a reaction and does it matter to the final yield?
Charlie said on Sat, 4 Dec 2021 at 22:01...
BTW, I felt this prep went much smoother, despite the problem with the crystals.
No noxious fumes, no frantic moments, the reagents chilled while doing other things, the pump was set and forget, etc. I felt that I had a much better idea what to expect.
Much, much, much smoother than the first batch where I spent all day and had frantic/panic moments at times and spent the next day feeling the effects of breathing noxious fumes.
Nitritespecialist said on Sun, 5 Dec 2021 at 14:43...
@Charlie: here's a file from 1914 detailing some of the findings of chemists of the period regarding their studies of amyl nitrite. I believe it's a two part report....and the other will have to be googled.
It's called :amyl nitrite; its preparation, tests and purity.
It mentions various ways to make AN.....apparently at the time, there wasn't consensus on the best way. They stated in this report that the sulfuric acid/sodium nitrite method was good enough for scientific work but not for scaling up to commercial application. They mention some of the possible impurities and properties of the various nitrites. Might be an interesting read.
The Professor said on Sun, 5 Dec 2021 at 17:26...
I'm glad that the prep went smoothly for you. One thing I wanted to ask you about. You mention putting the pump tubing just under the water line. Do you mean just under the surface of the liquid (which contains alcohol, water and NaNO2)?
I only all because the pre-chilled solution of H2O has layers, associate on top and water/NaNO2 on bottom. Best practice is to pump into the bottom layer
The Professor said on Sun, 5 Dec 2021 at 17:38...
Re the file on the above posters hard drive. It's an obsolete work from 1914 that Ken tried to impress the members of Reddit with for years ago.
I doubt that you have access to the link he posted, which is on his own machine, but it is available elsewhere. The ideas on our have been debunked as irrelevant with today's procedures and chemical availability.
Chemicals are much more pure today then they were back when people were just discovering many of these properties.
It remains to be seen who this new imposter using lens screen name really is, but he seems to be on some type of campaign to sabotage DIY
Nitritespecialist said on Sun, 5 Dec 2021 at 18:34...
Once again it's the nutty Professor's attempt to discredit the REAL chemists who were professionals and worthy of published journals. Amyl nitrite was discovered in the 1860s and by 1914, a lot was known about it. What does it hurt to read historical accounts from so many chemists who were instrumental in bringing amyl nitrite into the world of medicine? The Professor has always been afraid his few chosen disciples will turn on him or doubt his "know it all approach" if they read all the various sources available online, which is exactly where I got the file...not from my hard drive.
These chemists were interested in making a "pure" amyl nitrite as well as testing the properties of the various nitrites. The Professor has NEVER been interested in making a pure nitrite, because he has always blended his alcohols, which means he has no idea what the individual properties are of each distinct nitrite...and yet he claims to know it all. As a scientist and hobbyist chemist, the Professor has no authenticity.
Nitritespecialist said on Sun, 5 Dec 2021 at 18:41...
I listen to whatever the Professor with a grain of salt. You have to doubt so much of it, especially when he presents his methods as the BEST and ONLY way....pier reviewed and all. He constantly claims he makes 95% nitrite, but he NEVER m akes a pure nitrite. They are all blended alcohols, from the butyl group. He used to include isoamyl alcohol in his blend, but decided it made his blended poppers too weak, even though amyl nitrite is much less inclined to give lingering side effects. The Professor has never even admitted that the butyl group can give terrible lingering side effects as the price one pays for a more active nitrite. He's totally biased and one sided and throws caution to the wind, hellbent on selling his butyl poppers despite the cost to the human consumer.
Charlie said on Sun, 5 Dec 2021 at 19:57...
Prof, in response your question, I am placing the dropping tube just below the level of the bottom layer that contains just the sodium nitrite and the water. This time, I specifically chilled the sodium nitrite and water separate from the alcohol so that I could place the dropping tube at the best level to start. After chilling the sodium nitrite and the water, I placed the dropping tube ~1 mm below this level. It was after this that I added the alcohol (and noticed the 10C temperature spike mentioned earlier), which reached up further along the outside of the dropping tube.
I believe this is in line with your post which says I should pump into the bottom layer.
This time, the larger diameter (28 mm OD) tube dropped the drops neatly into the solution, rather than running down the sides of the tube. In between last batch and this, I managed to level out the freezer perfectly probably negating the need for a larger dropping tube. However, it was still easier to see the drops fall since the tip of the dropping tube just poked through the end of the rubber stopper at the top of the tube. I hope that makes sense.
P.S. Do you have an elementary explanation for the temperature spike when I added the alcohol to the sodium nitrite/water? ty
Hanky Code said on Sun, 5 Dec 2021 at 20:10...
the above posters hard
"above poster"..hmmm....who is this guy and what is his agenda?? because he seems to be copying Nitritespecialist's original posts and dropping in recommendations, so trading off Nitritesspecialist's reputation
on another thread he was attacking artisan poppers and is constantly praising pentyl
Professor? do you know?
The Professor said on Sun, 5 Dec 2021 at 20:19...
Your results have been fantastic so far, IMO; you attained reaction control very quickly, and now can tweak to your heart's desire
Some people NEVER attain control of the reaction, so you are several steps ahead of the average bear.
Ken's imposter seems determined to get you to fail and give up for some reason.
There's nothing wrong with research, but when you start to claim that, for example, pyridine and nitric acid are POSSIBLE impurities in an alkyl nitrite because it was found in a bottle in 1914, that's when one's personal assertions overwhelm their understanding
with today's procedures, there is no chance of pyridine or nitric acid unless they are intentionally introduced (or in the case of nitric acid, if the reaction is too fast and aerobic, which is the maker's fault).
I haven't mixed the ingredients like that (chilling alcohol separate from sodium nitrite and water) Sodium nitrite typically has an endothermic reaction, which would temporarily decrease the temp.
The only situation i'm aware of that requires care when mixing the initial solutions is if you are using sulfuric acid; Sulfuric is very desiccating, and will scorch the alcohol is they are dumped together; you have to introduce them to each other drop-wise
The Professor said on Sun, 5 Dec 2021 at 20:21...
I have no idea; he/she is getting SOMETHING out of it, since he/she persists, but what that might be?
Charlie said on Sun, 5 Dec 2021 at 20:28...
TY Prof. I am going to give it another attempt shortly and aim for -12C to see the effect on the crystallization problem I encountered. Do you know of any effect on the yield if it freezes over?
The Professor said on Sun, 5 Dec 2021 at 22:16...
I haven't had that issue arise, but I doubt that it would damage the vapor
Nitritespecialist said on Sun, 5 Dec 2021 at 23:09...
The Professor thinks that even the patent registered in 1958 is too old and too WRONG to take seriously. It clearly speculates that potassium carbonate can preserve amyl nitrite 10 fold and it says the reason is likely that Kcarb functions as an acid sink for nitrogen dioxide and nitric acid which forms as the alkyl nitrite degrades. As a know it all hobby chemist, the Professor simply thinks he's better than all other chemists combined.
Nitritespecialist said on Sun, 5 Dec 2021 at 23:13...
Once again, the Professor refuses to acknowledge the strong risk of lingering side effects when using poppers from the butyl group. Charlie has even stated he had a bout with low blood pressure from some of his home brew butyl, yet the Professor refuses to warn inhalers of the additional risks associated with the butyl group.
Nitritespecialist said on Sun, 5 Dec 2021 at 23:27...
It is shown that the stability of amyl nitrite ampuls can be greatly increased by the addition of various substances—including potassium carbonate (solid), trisodium phosphate (solid), magnesium oxide (solid), pyridine (dissolved), and diphenylamine (dissolved). The mechanism of stabilization appears to involve behavior of these agents as sinks for nitrogen dioxide and/or nitric acid produced during the breakdown. The degree of stabilization achieved suggests that the shelf life of the nitrite ester can be readily prolonged as much as tenfold as compared to present commercial products.
This is from a patent filed in 1958. Of course the Professor has debunked every single patent regarding alkyl nitrites going all the way back to the initial discoverer. He's the self professed world's expert.
Hanky Code said on Sun, 5 Dec 2021 at 23:44...
He's the self professed world's expert.
remove the "self professed" and you might be right for once..
my question to you "Nitritespecialst (version 2)" is why you are copying and pasting old posts and bad-mouthing butyl....
Charlie said on Mon, 6 Dec 2021 at 01:24...
I'm not sure what caused the low BP that I experienced about a month ago from my last batch. It could have been that I didn't neutralize the remaining acid long enough so I was inhaling hydrochloric acid left over from the prep, which is my best guess at this point. It could have been the nitrite, but the cough that I experienced also led me to conclude that it was probably from acid.
Charlie said on Mon, 6 Dec 2021 at 01:26...
Correction: excess mucus, which was causing a cough.
Nitritespecialist said on Mon, 6 Dec 2021 at 10:52...
@Charlie....Of the thousands of brews I made of the various nitrites, the amyl group is the only type that NEVER caused lingering low blood pressure, the type where you cannot possibly take another whiff because you've hit death's door.
Moreover, of the 3 types of nitrites I bought from large chemical makers, such as Sigma Aldrich, both isobutyl and n-butyl made my blood pressure cave, but the isopentyls did not. The Professor says its ONLY due to a commercial nitrite of 95% purity being too impure to inhale, but yet doesn't explain why ONLY the PENTYL group caused no low blood pressure symptoms.
@Hanky....go educate yourself about blood pressure and how it's vital to life.
Nitritespecialist said on Mon, 6 Dec 2021 at 10:58...
@Charlie....it will be interesting if you can consistently make N-butyl so that it NEVER caves blood pressure. I am not saying it's impossible, but I think it's very difficult. Whereas, I've been hitting my most bottle of JJ Black from LRM, the real experts, ten times a day for the last 4 days and it's nothing but FUN in a bottle. Zero side effects and total ass fuck joy. I did take a cue from the nutty, vindictive Professor and added a lot more Kcarb upon opening. It sure didn't hurt. I've been loving it for 4 days, during which time it's constantly been exposed to air at RT, something he admonished me for doing when he sent one of his toxic poppers.
Nitritespecialist said on Mon, 6 Dec 2021 at 20:07...
Air & Water Reactions
Highly flammable. Decomposes on exposure to air, light, or water. Many of the decomposition products, but not all, will be colorless flammable toxic gases. Insoluble in water. Reaction with moisture in air or with water produces nitric acid.
Special Hazards of Combustion Products: Toxic oxides of nitrogen are formed.
Behavior in Fire: Containers may explode. (USCG, 1999)
The above concerns amyl nitrite is from noaa.gov.
Nitritespecialist said on Mon, 6 Dec 2021 at 20:15...
Of course the Professor will debunk any source not his....and claim that there can never be traces of nitric acid in poppers and that it cannot form as a result of degradation. Certainly Nitrogen dioxide gas is evolved during synthesis and can be found tinting the popper yellow. The Professor claims nitrogen dioxide cannot turn into nitric acid during synthesis or during degradation of the popper once bottled.
Charlie said on Mon, 6 Dec 2021 at 20:30...
@Nitrite: I haven't used my last batch as hard as I did after the low BP with the previous batch (immediately after the prep), so I cannot know for certain if this batch would do the same thing after an extended use. I do not feel low BP or excess acid (mucus), but it could be the result of taking it easier as is normal for me. I do not usually ever use poppers for an hour so that incident could have been my own metabolism too and unrelated to the prep. I will be honest in the future if it happens again.
Charlie said on Mon, 6 Dec 2021 at 20:32...
I will soon need additional HCl and it does not make sense for me to use the same supplier. If the 37% HCl in the prep is being diluted with water, would it be OK to use 32%/20 degree Baume technical grade vs 37% (12.1 mol) ACS-grade and adjust the amount of water added? The 32% is described as American made, prime, virgin material.
Charlie said on Mon, 6 Dec 2021 at 20:44...
I also have a question about potassium carbonate. I am using lab-grade anhydrous potassium carbonate, which presents as extremely tiny granules or round pellets. I noticed that it has broken down in the nitrite to a powder that appears heavy. What does it mean that it has changed form and apparently broken down from its dry form?
The Professor said on Mon, 6 Dec 2021 at 23:35...
Ken's imposter seems to be implying that nitric acid is possible in a chemical prep that proceeds anerobically because he read that the national oceanographic institute finds it in reactions.
This idea has already been debunked guy; you must have cut-and-pasted right by it.
The salient point, pasted below from the last time he cycled through this lie, is that, if prep'd as specified in the guide, the entire reaction will be anaerobic.
The absence of O2 changes everything; in the case of atmospheric clouds (floating in O2) nitric acid develops as acid rain. Why does it happen in the air but not in the lab? Because O2 provides the activation energy to allow the reaction to proceed, whereas an anerobic dropping prep won't have that activation energy so there's no nitric acid generated.
"YES, the chemical formula that he read said that NO2 and H2O (nitric oxide and water) can yield HNO3 (nitric acid), but what he fails to understand, repeatedly, is that the specific heat of formation required to do that (117 kJ/mol) is just not present in the two phase liquid preparation. The nitric acid preparation happens at about 9 times atmospheric pressure and 500 or so Kelvin.
His riposte, that 'acid rain' happens, is laughable.
Yes, acid rain happens. Why? becauue a square meter of atmosphere is bombarded by at least 1 kilojoules of solar radiation every second in full daylight.; a cloud that's larger than 100sq meters, and saturated with both water vapor and NOx WILL have enough energy to form (at least partially) Nitric acid.
Again, when you point your finger, you have three more pointing back at yourself.
This member's entire library consists of falsehoods, outright lies and mis-comprehensions"
The Professor said on Mon, 6 Dec 2021 at 23:41...
the main reason i but the highest concentration i can is because HCL is more stable at higher concentrations. That said, there's not much of a difference. The reason to dilute HCL is mainly to control reaction speed; the peristaltic pump seems to be a winner in that regard. If 32 is preferble to you, go for it (you';ll have to recalculate the molarity)
Potassium carbonate will change with use, yes; it eventually turns into a pink paste like substance.
Charlie said on Mon, 6 Dec 2021 at 23:57...
This fourth batch has been on molecular sieves and potassium carbonate for 3 days. After several whiffs over 15-20 minutes, it seems to have some undesirable after effects. It has decent effects during use (especially smooth muscle relaxation), but afterward I seem to feel light-headed and the tips of my fingers seem to be turning bluish. I feel like it is headed toward the effects of my last batch immediately after prep.
Do you have any ideas? It seems to smell decent, maybe just a little acidic, but not so much that it is repulsive. I have been adding 1 g potassium carbonate each day over the past 3 days to the yield (~40 ml) in hope of reducing any residual acid.
TBH, I am feeling discouraged at this point because the last thing I want is to feel worse afterward and that this has been a failure for me.
Charlie said on Tue, 7 Dec 2021 at 00:35...
Prof., I am debating whether to sink more resources at this stage (been rapidly discouraged), but in the event that I choose 32% HCl, do these numbers look correct?
HCl 12.1 mol (37%)
1 mol = 82.7 mL
1.1 mol = 91 mL
+ 20 mL distilled water = 111 mL total solution volume
HCl 10.172 mol (32%)
V = volume of moles needed ÷ molar mass
V (ml) = (1/10.172) * 1000
1 mol = 98.4 mL
1.1 mol = 108.2 mL
At this point, should I add 2.8 mL distilled water to the 1.1 mol of 32% HCl to bring the volume up to 111 mL as when using the 37% HCl?
Charlie said on Tue, 7 Dec 2021 at 07:32...
...or do you believe that diluting the HCl is not necessary for prep with a peristaltic pump?
The Professor said on Tue, 7 Dec 2021 at 16:47...
Blue fingertips so quickly is not a good sign. If it's not a residual acid issue (you seem to be neutralizing properly, it's hard to tell), then it may be that your metabolism is getting more NO than it can deal with.
Personally, we haven't turned blue, even when our sessions go very long. The blue fingertips is a temporary cyanosis brought on by the poppers interfering with hemoglobin activity. If this happened to you after a long while, that would be one thing, and possibly due to excess acid, but if it happens so quickly it's just more likely that Butyl is too strong for your body to process.
How to tell the difference? Well, I went about this backwards. I started with amyl alcohol, and once I had that level of reactivity down, I moved up to the Butyl group, which was much more suitable for me.
Two things to try
1. Ensure that you are neutralizing properly (it seems like you are already doing that)
2. Slowly reduce the HCL in the prep, about 5% (0.05 mole) at a time until their is just a hint of blue remaining in the waste phase (you'll know if you go too far when the yield starts to reduce, e.g. 1.15 mol should have the same yield as 1.1 because the alcohol is the limiting reactant, but at some point you'll start getting less yield. That would be the absolute least amount of HCL to use.
If that doesn't work, then it might be time to try one of the less reactive nitrites. The procedure should be the same
Nitritespecialist said on Tue, 7 Dec 2021 at 20:07...
@Charlie....after ten years of making nitrites and coming to the conclusion that the amyl group was the safest to make....with least bad side effects...lo and behold the Professor seems to be steering you there. I think n-butyl nitrite has potential to be fun, I just don't know how to make it well enough to inhale. On a side note, the 2nd bottle of JJ Black I opened was too acidic and I had to wash it and rebottle it. Acid seems to mute effects, give a hoarse throat, and burn/sting nostril skin. I don't know what type of acid(s) are present, but acid never seems to be good.
Nitritespecialist said on Tue, 7 Dec 2021 at 20:13...
@Charlie....and remember I bought 25mls of 95% n-butyl nitrite from Sigma Aldrich....Within 5 minutes of whiffing it, my BP collapsed. I noticed my finger tip had turned yellow and the fluid stung a bit so I washed and dried it. 100% better after this with no collapse...but it evaporated quickly so didn't get to savor it long. The residual popper with Kcarb in it smelled VERY VERY sweet like bananas. That residual odor is very distinct and might point to a well made N-butyl popper. It didn't smell so much like bananas at first....I'm speaking of the residue left in the bottle, which could be a tell tale sign that the popper started out pure enough.
Charlie said on Tue, 7 Dec 2021 at 20:17...
Last night, my other half tried this fourth batch for the first time and said that they were very much improved over previous attempts. Now, I don't know what to think exactly... Granted he didn't use them for long, but it was an encouraging sign to get positive feedback, rather than my own biased assessment. I still do believe though that either this is too reactive for my metabolism or there is something in them that shouldn't be there, like residual acid. Or it could all be my mind playing tricks after the low BP incident last month. I really wish I knew exactly what alcohol or combination of was used in commercial poppers that worked for me in the past.
I have been wanting to try amyl, so it is probably one of the next logical steps to try and see if there is any difference for my metabolism.
In preparation for my next batch, I attempted to freeze my beaker in the 8C Pyrex. In hindsight, it was only a matter of time before the beaker cracked! On to remedy the ice bath situation. I believe I will try ice-salt slush in the freezer with the beaker clamped down.
I believe that this last batch was neutralized better than previous batches. It was mighty cold during neutralization so the baking soda clumped especially well. It is amazing how much temperature affects the clumping. I made sure to agitate rapidly for a good 2 minutes and I noticed bubbles this time. I did not notice any "fizzing" exactly like Mentos into soda, but rather I saw bubbles. Bubbles are good, right?
I noticed that the solutions turned color to green and blue at about the point that 3/4 of the acid had been dropped. Does this information itself provide any indication of the extent of the reaction completion and how much more acid is required to use up all the alcohol?
I believe I am already using 1.1 mols of HCL in my preps (the numbers posted a few comments above). Based on your post, it seems that I should not go below that.
Nitritespecialist said on Tue, 7 Dec 2021 at 20:22...
@Charlie....I suspect the butyl alcohol source might be important....the best source I got was from TCI....other sources smelled different and I never got a string of good butyl nitrite as I did with TCI's butanol.
Charlie said on Tue, 7 Dec 2021 at 20:31...
I do not recall at the moment, did you ever try blends of amyl and butyl? Were you ever able to determine a concentration of butyl that did not have negative effects for you?
I was curious yesterday about your JJ Black posts and went back to read. I saw that you had somewhat mixed experiences between the bottles. How are they now that some more time has passed?
The Professor said on Wed, 8 Dec 2021 at 00:19...
There's very little that can go wrong at such low temperatures; there just isn't enough energy in the apparatus to allow side reactions, and your reaction speed seems under very nice control. The only thing two things I can think of I already mentioned (neutralizing and reducing acid molarity).
As it is, you are using 1.1 mol of HCL, 1.1 mol of NaNO2 and 1 mol of alcohol?
That's what I used when I gen'd up a quick peristaltic pump prep to follow along with your trials. It ended up perfect (for us), but I am getting plenty of foaming during neutralization.
The amount of baking soda the guide suggests should neutralize up to 20% excess HCL, and I haven't had any issue at all; the nitrite smells very very slightly of ginger ale, never a hint of distress during inhalation, and the effects are fantastic.
Since I haven't been having any issue with neutralization, i didn't bother with titrating the HCL down, but that's something that can be done easily enough (posted above).
If your liquid seems smooth and fresh to inhale, but you still get the weak feeling, then it's most likely too strong for you.
Charlie said on Wed, 8 Dec 2021 at 01:16...
You mentioned that you got plenty of foaming during neutralization. I do not recall seeing that during neutralization. I used brand new baking soda with an expiration date a few years from now. I saw an emulsion and bubbles, but never what I would consider foaming or fizzing. I wonder if it's the yield, the baking soda or process... Hmmm...
I am using 1.1 mol HCL, 1.05 mol of NaNO2 and 1 mol of alcohol. Could that 3.4 grams of NaNO2 difference between what you used (1.1 mol) and what I have been using (1.05 mol) mean something?
In general, what would happen if there is not enough NaNO2 to satisfy the HCL and alcohol?
Nitritespecialist said on Wed, 8 Dec 2021 at 01:40...
@Charlie, I had two sessions with my newly washed and dried JJ Black from LRM. Improved odor...and the effects are much improved...incredible ass effects. So there is gold in the bottle but it was tainted with acids and who knows what else. I put a lot of KCarb in for one day with little improvement...which is why I decided to wash it...The 5 bottles had different lot numbers but I expect I'll be washing each one just to maximum effects and longevity.
I have mixed alcohols with mixed results. You can't judge a brew based on one brief session....you have to see how it ages too....if it doesn't have much longevity....only lasting a day or two, it's probably tainted with impurities. The LRM bottles at least have enough active ingredient that washing them doesn't kill them and I've had them last weeks afterwards.
The Professor said on Wed, 8 Dec 2021 at 17:46...
Let's take a look at the reaction again from the guide.
Example is Butyl alcohol
The reaction is actually quite simple. Reactants are introduced to a solvent medium (H2O) and dissociate into cations
and anions; the ions then re-combine to produce the desired compound. The following example uses n-Butyl alcohol
and Hydrochloric acid (the reaction is actually a two stage process).
HCL + NaNO2 = HNO2 (nitrous acid) + NaCL (table salt)
HNO2 + C4H10O = C4H9NO2 (butyl nitrite) + H2O (water).
These are balanced equations, so an equimolar
amount of all reactants will fit (theoretically). Your chosen method of synthesis (which reactants you pre-mix/what
order, etc.) will determine the actual amounts, but I find it useful to treat the alcohol as the limiting reactant, and bump
the NaNo2 and HCL up to 1.05 to 1.10 mole. this is a starting point, and you will determine the preferred ratios your
NaNO2 and your HCL in the data logging section.
Your question is regarding NaNO2 molarity.
Looking at the equations, it seems to me that NaNO2 is responsible for providing nitrous acid that goes on to combine with the alcohol to nitrosate it.
With a lack of nitrous acid, there will be some un-reacted alcohol remaining in the solution.
I suggested that you reduce the acid because your waste phase was slightly blue (deep blue would indicate excess of NaNO2) so it seems that you've locked down the NaNO2, and as long as you store it well, it will stay viable for a long time.
The remaining tweak, as it seems to me (and I'm going by what I think from not being there so I'm not a very viable witness) would be too limit the HCL until it starts reducing the yield.
All of this is covered in the days logging section (which is intentionally obscure in that it shows you a path of interest for your own further explorations.
I don't give dot by dot, color by numbers instructions. For one thing, I think that would be annoying to try to tell somebody what to do.
The guide is really trying to teach people how to fish, rather than providing them meals.
Charlie said on Wed, 8 Dec 2021 at 18:19...
I really appreciate your time and energy helping me. You have really pointed me in the right direction countless times and I am eternally grateful for your help.
I appreciate your approach and very much respect your method. Please forgive any outright direct questions as they are not coming from a lazy side, but rather the unsure and constantly-questioning side of me. Since this is all so new for me, I feel that I am fumbling at times, even with your extensive help. Trust me, will re-read your post many, many times in an attempt to digest it to the fullest extent!
Nitritespecialist said on Wed, 8 Dec 2021 at 22:06...
The basic chemical description of what is supposed to be happening in the pot when making an alkyl nitrite is somewhat misleading because it doesn't mention all the possible problems that could lead to side reactions and incomplete reactions. And it doesn't address how to solve all these problems. When is the reaction complete? You certainly can't tell by looking at the pot unless perhaps you've tested your crude yield for purity and correlate those results with how the pot looked when the yield was harvested/tested. A blue/green color certainly indicates the presence of nitrous acid, but it doesn't tell you much else. It doesn't tell you what the purity level is and what all the impurities are besides the reaction water, base alcohol and the acid used. The best you can do without a tried and true indicator is delay the harvest for a long time, in hopes that at least the reaction is as complete as it's going to get. But since the reaction reaches a point of equilibrium, the reactants may never fully react to form the expected product. There are methods to force a reaction towards the product.
Usually it means changing one of the conditions in the pot. Even still, you'll never know what's in the crude yield or processed yield without an accurate way to analyze it.
The Professor said on Thu, 9 Dec 2021 at 00:29...
Not being able to neutralize your yield had me flummoxed. It should look like this.
Charlie said on Thu, 9 Dec 2021 at 03:05...
TY Prof for the link. I've never seen any fizzing as shown in the video. I have seen an emulsion and I have seen bubbles, but never fizzing even with the new baking soda.. I tested the baking soda with just some vinegar and it is certainly viable.
This leads me to furthrr wonder what's happening....
I am beginning to believe that the cyanosis is probably because the n-butyl is too reactive for my body. I have some n-propyl so I did a quick 1/2 mol batch for a little experiment, using the same exact process and reagents as the n-butyl prep - except for the alcohol adjusted for molarity. Got significant cyanosis within a minute or two - just a couple whiffs was enough for blue fingers, toes and lips. I expected cyanosis so I did not overdo it, but the speed with which I got cyanosis was a little alarming. This led to me since believe that the more reactive alcohols could just be too much for my metabolism. I believe that I should probably try the amyls and see if they are better for my body. I have been going back and forth for days whether to first try isoamyl or n-amyl. Any recommendation?
Charlie said on Thu, 9 Dec 2021 at 03:21...
On the upside, the n-propyl prep gave me an opportunity to test out my new ice bath method: 200 g table salt and 1L water frozen overnight to -18C - placed in a 64 oz. rectangle food storage container with the reaction taking place in the chest freezer. Didn't use much salt and didn't have to change the ice. Kept the reaction nice and cool to -10.4C in the end. I started at -14.6C. Next time, I plan to start the prep when the reagents are at -16C. That way, it will end up at -12C. No crystals frozen in the yield layer this time.
Charlie said on Thu, 9 Dec 2021 at 06:45...
Forgot to mention:
The n-propyl nitrite had incredible effects during use for those few brief minutes. For those few minutes, I believed I had found the holy grail! BUT, it was the after effects that were too bad unfortunately. All was expected though.
It smelled a little like acetone - I believe you said this before Prof. It evaporated incredibly quick. A few milliliters evaporated within a couple minutes. Did not smell acidic at all like my preparations of n-butyl (can't yet understand or explain this because the preps were identical). The smell was actually pleasant.
However, won't be doing that again...for obvious reasons.
The Professor said on Thu, 9 Dec 2021 at 18:33...
Oh boy, n-propyl nitrite is more reactive than the active ingredient NO,; it definitely adds undesirable effects to the mix. Yes, once things get to a certain reactivity, it all starts to smell like acetone. Tert-is as high as I would suggest that anybody go. It has an acetone like smell, but a bit different, and the effects are still within the realm of the dance between vasodilation and heart rate that a nitrite does.
Even as a top note in a blend, n-propyl packs to much for me. Somebody in their twenties maybe,
There's no method that I know about that shortens the learning curve any more than I've already done.
You have achieved control of the reaction more quickly than any maker I've worked with. All that remains is tweaking the prep to achieve a preferred embodiment for your apparatus.
The troubles with neutralizing really have me stumped, but the way forward seems to be reducing HCL
Personally, of the prep and stabilization is adequate, then the only difference between n-Amyl and isoAmyl nitrites are the reactivities. IsoAmyl is slightly more reactive, so it will require more attention than n-amyl. N-is very easy to prep and stabilize, ok have no experience with cyclohexyl nitrite, but it might be even easier to make since it's very low reactivity.
I couldn't tell the difference, in effects, between N-and isoAmyl (they are within 5% of each other) except for aroma.
IIRC, sec-amyl gets close to n-Butyl
In reactivity! if it turns out that Butyl is too much for your metabolism, that's always an option
Charlie said on Thu, 9 Dec 2021 at 19:12...
Ty Prof. I sincerely appreciate all of your time and energy.
I will work on dialing in the HCL. During the n-propyl prep and 4th batch of n-butyl, I noticed brown NO2 beginning to accumulate in the dropping tube the last couple minutes of the prep. I know we briefly discussed this before. I also recall reading that a little NO2 is a good indicator at the end of the prep because it could signal that most of the alcohol has been consumed. Maybe this is also a good signal that I could probably dial back the HCL slightly? I've also noticed that the solution(s) begin to cool ever-so slightly at this stage, maybe signaling that the reaction is slowing (I know we also discussed this before). This cooling, with the gas accumulating in the tube, may be trying to tell me something?... I am learning as I go here and trying to watch for visual clues as much as watching the data.
Although the cynanosis from the n-propyl was unpleasant, I feel that the experience provided me with another data point about different alcohols. It showed me that changing just one input can change the yield significantly. It seems that it opened my eyes to reactivities, as well as provided me with more data points about my other reagents. It wasn't all for nothing. The evaporation also reminded me of alkyl nitrites that I've bought in the past that would evaporate quickly. I am just starting to put pieces together with the data and experience...
I am very interested to try different, less-reactive alcohols and see how they work for my metabolism. I have not found a source for sec-amyl so that may be down the road after iso or n-amyl. TBH, I experienced cyanosis before with some commercial poppers but was never able to nail it down because of my lack of understanding. However, with my recent experience, I'm now beginning to form some theories.
The Professor said on Thu, 9 Dec 2021 at 22:55...
back in the day, there was a brand called 'blue boy'.
The cyanosis should be temporary (20 minutes or so), unless your body has that mutation that doesn't allow it to process methemoglobin effectively. What's really troubling is if the nitrite drops your blood pressure to the point of nearing unconsciousness. Anything that makes you feel weakness/fatigue should be avoided.
Nitritespecialist said on Fri, 10 Dec 2021 at 13:38...
@Charlie....you are discovering everything I had learned on my own years ago and have been posting online for years. This is why I frown when
people ask for the "strongest" possible poppers. The strongest means it's the most toxic. The last isopropyl nitrite I made had incredible effects for 5 minutes...and then the bottom fell out and I couldn't take another whiff. This apparently is the nature of the beast because you have experience similar bad effects. The rare blind case seems less important to me than the fact IPN is just too damn toxic overall.
You are also discovering what I discovered...that N-butyl nitrite is hard to make. It almost always turned out disappointing for me with toxic effects. I had a string of successes where it was good. That's when it smelled sweetest and it didn't give the dreaded toxic effects.
N-amyl nitrite doesn't give the cough reflex or degrade into a bad odor like Isoamyl nitrite does. It's an easy decision there.
Nitritespecialist said on Fri, 10 Dec 2021 at 13:40...
@Charlie.....I also had problems neutralizing the acids to where it didn't burn my skin or smell acidic.
You might try sodium carbonate(washing soda) instead of baking soda. If it's anhydrous, it can work as a preservative as well.
Nitritespecialist said on Fri, 10 Dec 2021 at 17:04...
@Charlie....I'll buy some of your n-amyl nitrite if you ever get to the point at which you are satisfied with it. LRM isn't reliable enough especially since retailers are selling old product.
I may resort to making it again...since even though there was variation, it didn't have the ill effects that the home brew butyl group did.
I think it's important to make it as dry and acid free as possible for maximum good effects.
What I think accounts for the variation in odor and effects is that I was bottling home brews that were already in various stages of degradation. The various stages of degradation, which are inevitable even when bottled 100% pure, all cause changing effects and odors or perceived variation. The old LRM poppers I was sent and have been using are giving off and unpleasant effects and they don't smell active. This would be expected of degraded poppers.
Charlie said on Fri, 10 Dec 2021 at 19:15...
Yes, straight n-propyl nitrite was not pleasant afterward. During...amazing and I thought I found the holy grail like I said. Then I looked dead from cyanosis. Took too long to recover.
I also have some different n-butyl alcohol that I am interested in trying. I have been sticking to the same reagents for the first several batches because I wanted to make sure that I dialed in the process somewhat before I started changing the variable inputs. Will be interested to see if changing the n-butyl manufacturer changes the yield.
I appreciate the suggestion/reminder about washing soda. Is the A&H dollar store variety OK or do I need to use the type that is 10x the price that says it is free from everything? I realize the A&H variety does not come anhydrous, but for neutralizing purposes is it OK?
Seems I was overhasty and will have to order some n-amyl later as I ordered some iso-amyl. I was going back and forth between both for days. I've been hesitant to continue to throw in resources in case things don't work out.
I was reading through my personal notes that come from multiple sources. I want to make sure I understand any differences between n-amyl and iso-amyl. I recorded the following about n-amyl:
-any of that the amyls are comparatively weak and irritate the throat more than others
-may get headaches during the session and may feel very tired the next day
-hard hangover with medium recovery
-may get blue nails and blue lips due to lack of oxygen
Is that wrong about n-amyl (and very well could be)? I didn't have any of those points listed under iso-amyl.
Nitritespecialist said on Fri, 10 Dec 2021 at 20:07...
@Charlie.....I used A&H washing soda and it seemed to work OK. I suppose it could be heated to make it anhydrous for preservation purposes as well. I read one tip to tell when you are done neutralizing....is to test the pH of the neutralizing fluid after it's used for neutralization - supposedly after the emulsification with the nitrite and subsequent separation into two layers. Apparently, when it tests neutral, the nitrite is sufficiently neutralized.
I have used TCI one pentanol the most, but have also used isoamyl alcohol. I only found the isoamyl alcohol to give me a cough reflex. I didn't buy any pure n-amyl nitrite to compare to isoamyl nitrite solely because of the extreme cost difference. So I can't say for certain how the two compare, except to say that my n-amyl brews never developed the same sort of funky, unpleasant odor that my commercial isoamyl nitrite did. I think the best anecdotal way to tell if an n-amyl brew is fairly pure is to see how long it maintains potency and a decent odor when it's stored with preservatives. I think if it lasts weeks, it's more pure than one that only lasts a few days if everything else is equal.
I don't think amyl nitrite is "weak" when it's fresh and supposedly pure. As far as I know, none of the nitrites will sustain ass relax, for example, without fairly frequent hits. With the amyl, it was easier to take frequent hits because it didn't cause the toxic effects. I also suspect n-amyl nitrite is more likely to give a surreal dreamy, euphoric effect once it has the proper composition.
Charlie said on Fri, 10 Dec 2021 at 20:43...
I will update on my success or struggles with isoamyl after I have an opportunity to prep some.
Nitritespecialist said on Tue, 14 Dec 2021 at 21:13...
US Patent 7314948B2
This patent from 2008 makes it seem easy to make 99% pure butyl nitrite. They gave a bunch of variations on their method, using different temps, etc. and they always got around 99% pure BN....with about 1% butanol as an impurity.
They said the acid level should be no more than 1.01 moles per mole of alcohol, an excess leading to degradation of the nitrite. The SN could be as much as 1.20 moles an excess of 20%. They mixed the HCl and alcohol together first and then added 40% SN to this at various temps. At 0C, they got 99% purity, but not much greater than at 10C or at -10C. They provided various runs with close to 99% purity resulting....don't have a clue how they did this, but apparently, it's possible. What the critical factors are remains a mystery to me since almost all my BN was smelly bitter crap that tanked BP.
Nitritespecialist said on Tue, 14 Dec 2021 at 21:18...
@Charlie, they also say that their method creates a longer lived popper, presumably because it's more pure. When I tried this method....last Spring, I did manage to get some longer living amyl nitrite.....I ordered more pentanol and will give it a go again, although, I would rather buy it ready made.
Charlie said on Wed, 15 Dec 2021 at 09:07...
Ty Nitrite. I'll look into it more. Specifically, the proportions interest me. I'll have to go back and find those threads.
I recall reading quite bit a couple months ago when I started about dropping SN. Maybe I'll have to give it a try for kicks.
Based on my notes, it looks like you may have tried the method of dropping SN using amyl alcohol? It looks like another user, Jacko, also commented on the process. I know there was some discussion about how dropping SN introduces more oxygen into the chamber because of the faster stir speed. And the alcohol is in contact with the acid, among other differences to dropping HCL.
Now that I am just beginning to get more comfortable, I will give the other methods a try after I sort out my familiarity with the different reagents. Already tried different SN - didn't detect any noticeable difference. Already tried n-propyl alcohol with the aforementioned undesirable results. Next, will try amyl alcohol and then would like to try different HCL. Once I sort out the reagents to my liking, I will feel more comfortable experimenting with the process.
Nitritespecialist said on Wed, 15 Dec 2021 at 14:31...
@Charlie...the patent stated the mixing temperature of the alcohol and acid wasn't that important, BUT it wasn't clear to me if they mixed the two at once....or dumped one into the other. I am going to try to add both together more slowly, like two steady streams while mixing. They also weren't clear as to whether they used two streams, one of the al/acid and the other of the SN solution, entering the pot at once. What stood out as clear and different was the acid amount....the ideal was 1.01 moles HCl, just a small amount over a perfect balance. They said any more acid leads to by products and degradation. They said they could leave the yield in the pot for days even without much degradation,presumably because there wasn't a lot of excess acid used to degrade the formed nitrite.
The Professor said on Wed, 15 Dec 2021 at 18:13...
It's very puzzling to me why somebody would purposefully sabotage another's work.
I've watched, over the past week, the same, already disproven, ideas being offered. Rather than, once again, explaining the truth of the madness, I'm going to realize why popchef asked for the PopperMakers reddit an invite only forum.
That was some NOT to keep secrets from anybody. It was done to prevent people like Ken, sabbateurs, from interrupting and confusing an audience that
is probably not well versed in chemistry.
Charlie, you seem to have the process down excepting for the neutralization process.
This puzzles me, because it is a process that doesn't require any skill, save the ability to sprinkle a powder into a liquid.
The only other maker that I've ever worked with that had such trouble with neutralizing was Ken (the original user of that screen name you're talking to). He attempted to do it with baking soda, then washing soda, then slaked lime. His ideas about why became more and more wild.
The TL;DR is that I'm not in a learning environment here, I can't continue to work when my suggestions are swamped out by three times the amount of BS and repeatedly failed ideas.
I leave you with this. Neutralizing is essential. If fou don't learn how to do it effectively, you will likely experience the same string of failures, and end up with the opinion that anything more reactive than the Amyl's is junk or poison.
The guide shows you how to customize your prep for a bespoke experience, with a wide range of options between 72% and 99% reactivity. Ken is leading you in a direction that limits your options to 72% reactivity.
Charlie, if you want to get real advice from real makers, hit up our group, PopperMakers, on Reddit for an invite
Charlie said on Wed, 15 Dec 2021 at 20:53...
Nitritespecialist said on Wed, 15 Dec 2021 at 21:00...
Thomas Petrow, the Professor takes issue with every single alkyl nitrite patent I mention, without ever directly addressing the patent itself, other than to say every single method, except HIS, and every patent has been debunked. Mr. Petraus has had plenty of failures...all of which he keeps secretive so that others won't do what he always does....which is to attack everyone else's "failures", which in my case has more to do with seeking a very high standard instead of the shitty high he and so many others think are satisfactory. Some people might think the poppers I made were good, but my personal standard is high. It's odd how Thomas never has mentioned side effects he has experienced from both his own brew and OTC poppers. He certainly knows about these effects, but he won't tell anyone...
Nitritespecialist said on Wed, 15 Dec 2021 at 21:06...
Once again, Thomas has suggested that Isopropyl nitrite is OK, since it's more reactive than the amyl group. He has clearly stated that the amyl group is too "weak" and unreactive....and that any good popper has to be something other than amyl....stronger...more reactive....which includes the propyl group....which Charlie has clearly stated made him feel very unwell.
Nitritespecialist said on Wed, 15 Dec 2021 at 21:10...
Thomas Petrow doesn't care about consumers.....whereas my only concern is for the consumer. I believe consumers should be well informed of all the possible risks before they decide do something. It was I who warned others and Charlie about the stronger side effects, namely low blood pressure, that the butyl and propyl groups are more apt to cause. It's only a footnote for the Professor. He only mentions the downsides after he's got you sucked into his "methods".
Nitritespecialist said on Wed, 15 Dec 2021 at 21:16...
And for the record, the amyl nitrite I had been making for over 2 years was far better than the butyl/isopropyl I had been making. I only stopped because I got tired of the mess and LRM seemed to have a decent amyl nitrite...American makers are not making amyl and I don't want to risk the side effects of the butyl group.
GCP said on Thu, 16 Dec 2021 at 01:20...
you don't now what you're talking about; we have products made with 1-pentanol, isoamyl alcohol, n-butyl, isobutyl and some amyl/butyl blends.
something for everyone.
Nitritespecialist said on Sun, 19 Dec 2021 at 15:17...
@GCP....apparently that's a new offering because the Professor is definitely anti amyl.