Online amyl prep from published book.

Topic created by Anonymous
on Wed, 15 Jun 2022 at 21:34

Anonymous said on Wed, 15 Jun 2022 at 21:34...

AMYL NITRITE

Amyl alcohol (b.p. 130®) ... 15 g. (18*5 c.c.)

Sodium nitrite (powdered) ... 15 g.

Goncentrated sulphuric acid ... 9 g. (5 c.c.)

The amyl alcohol is measured into a 250 c.c. round-bottom
flask after which the sodium nitrite is added and the two are
thoroughly mixed. The mixture is cooled in ice and concentrated
sulphuric acid added drop by drop from a dropping funnel with
continuous shaking (one hour). In the later stages the addition
of sulphuric acid is made slowly owing to the tendency of
the reaction to become vigorous. After the addition of the acid
is over, the contents of the flask are taken in a separating funnel,
the upper layer of amyl nitrite is separated, and the lower layer
diluted with a little water in the separating funnel itself whereby
some more amyl nitrite is obtained, which is separated and added
to the main bulk. The amyl nitrite is dried over anhydrous cal-
cium chloride in the separating funnel, filtered into a clean distilling
flask (50 c.c.) and distilled. The portion coming over between
95-100® is collected, weighed and sealed in a tube. It is a yellowish
green liquid with a penetrating and sweet smell ; b.p. 99 ° ;
sp. gr. 0-87220". Yield, 13 g.

Notice how it takes an hour of addition just for 5 cc's of c. sulfuric, WITH SHAKING constantly...likely because the sulfate precip is so thick a stir bar won't work well.. The book is from the late 1930s or early 40s. It's similar to the Italian method provided by the person who uploaded the WikiLinks.

The Professor said on Wed, 15 Jun 2022 at 22:39...

I wonder in what way you are finding a similarity with your 'italian' method. Wasn't that the one that changed the traditional drop method from dropping acid to dropping nitrite?

If so, this prep is dropping acid, 2while the italian method drops nitrite.

In what other way are they simialar?

Uh, the prep calls for shaking instead of stirring. OK, so?

I see no mention of how long the reaction takes, and Sulphuric acid does cause that thick precipitate which bogs down a stir bar, but my question to you would be

If the product is shaken, not stirred, how in tarnation can sulphuric acid bog down the stir bar?

never mind, you;ll just sput another incorrect fantasy.

The reaction takes that long because otherwise the excess heat generated will consume the entire apparatus and boil off the reactants. a consistent and very slow drip speed is key.

Anonymous said on Thu, 16 Jun 2022 at 15:17...

I performed the aforementioned prep with one change. I used 15 mls of 35% sulfuric acid....auto acid. This should give about 5 mls of pure acid per the prep illustration.

I added no extra water to anything. I mixed the SN powder into the alcohol.

Cold ice bath and slow dripping of acid...about one drop every 5 seconds.

I saw orange brown gas form, but it stayed mostly on top of the reaction, perhaps replacing any O2 near the surface...as nitrogen dioxide is heavier than air.

Lots of precip/crystals. I thought it was going to be a total bust, but as I began to harvest the yield, and then add small amounts of water to the reaction flask, I got more and more yield....about 14-15 mls of final yield.

I washed in brine/soda 4 times.

Odor: slightly fruity, mild, aromatic, like a cleaning agent

Effects: pleasant...libido increasing, mild but marked, strong ass relax, mild euphoria. Does exactly what I expect it to without any weird or off effects.

So....it works, but it's SLOW.

Anonymous said on Thu, 16 Jun 2022 at 15:35...

I will post again to see how it ages. So far. 24 hours old, it's really good with no trace of off odor or effects. No acid....

Theory is.....the longer it preserves, with or without use, the more likely it was more pure OR it possessed a chemical composition that afforded longer shelf life...OR perhaps post processing was more efficient. I am betting it's more to do with the chemical composition coming out of the pot.

The Professor said on Thu, 16 Jun 2022 at 18:59...

I'll take that bet

and you lose

Nothing has changed since the LAST time (and time before that and ......)

decomposition rate is NOT a function of pre-existing impurities, and degradation does NOT increase exponentially

To Whomever is listening, Ken is a proven liar, saboteur and his 'theories' are Q-ANON level

He's going through a 'rope-a-dope' phase in which he regurgitates posts from the past (which have already been debunked) in some way trying to 'wear me down' , but the tactic is failing big time, as whatever crazy nonsense he spews makes him look foolish and dangerous.

In this case, the real answer is here:

temperature drastically affects decomposition:

https://imgur.com/gallery/jQKPwTs

Oxygen is bad news for Alkyl nitrite lifespan:

https://imgur.com/gallery/5os7OnO

Water will also kill alkyl nitrite quickly:

https://imgur.com/gallery/o7FurXp

In all of the above graphs, 4CC of gasses represents 10% of degradation.

NONE of the graphs (excepting fig 4 plot 3 showing stabilization) exhibit behavior that increases degradation as contaminants increase; that would require an exponential plot, and the graphs show linear responses.

now pay me! or are you so morally bankrupt that your word is worthless?

Anonymous said on Thu, 16 Jun 2022 at 20:58...

I tested again and it's excellent. Similar odor with very good effects....definitely has a cleaning agent, spic and span type odor...but VERY MILD.

I used a oxygen meter right after....amazingly...HR in the 50s and O2 92. Wow....this could mean the stuff I made was VERY RIGHT.

Anonymous said on Thu, 16 Jun 2022 at 21:03...

I have two 10 ml bottles. So far the first has shown very little evaporation and just a one bead of MS4 and a sprinkle of dry potassium carbonate and the one I've tested is spot on...excellent 24 hours later. Not a trace of acid or bitterness. My friend said effects strong after taking a tiny whiff.....but for me it seems pleasantly mild.

There was little water used in the prep....this could be why the popper could be more pure...perhaps the equilibrium was pushed further to the right, to a more complete product. Excess water inhibits esterification and sulfuric acid acts as a dehydrating agent as well.

Anonymous said on Thu, 16 Jun 2022 at 21:07...

There was only about 10 mls water used, coming from 15 mls of 35% sulfuric. I used 18.5 mls of alcohol and 15 grams of SN....so very very little water compared to what I typically use. And the prep actually called for no water....

During the reaction water is formed...so there will be some eventually.

The Professor said on Thu, 16 Jun 2022 at 21:13...

too bad it's all lies; his pulse-ox readings don't make sense, he's doing the 'sulphuric acid must be DRY with no extra water' thing, aqain.

another big yawn with no new content.

Those interested in the REAL science can always refer to the wiki, and join PopperMakers (a subreddit) if you need support for it.)

wiki:
https://nublu.maitriworks.org/files/Alky%20Nitrite%20Preparation%20wiki.pdf

Maker's forum:
https://www.reddit.com/r/PopperMakers/

Anonymous said on Thu, 16 Jun 2022 at 21:17...

Also, the prep said to add a little water to help with harvest/separation. I did and it helped a lot. Apparently, at this stage, when the reaction is complete...adding water doesn't hydrolyze the ester, but helps separate it from the sulfate crystals. The crystals will absorb the water and displace the ester, which is not soluble in water.

Anonymous said on Thu, 16 Jun 2022 at 21:19...

I hope this helps for all makers to at least try to make a reference sample that can then be compared to other brews using different methodology. Only then can one be more certain of any particular method.

The Professor said on Thu, 16 Jun 2022 at 23:21...

Apparently? The ester only hydrolyzes during prep?

That's completely wrong, of course, and in no way addresses any of the challenges involved in PowerPoint a reference standard.

The Professor said on Thu, 16 Jun 2022 at 23:22...

Prepping

Anonymous said on Fri, 17 Jun 2022 at 11:21...

I retested my NAN this morning and it's still delivering strong effects and good odor. No trace of bitterness, acid. Has a spritzy, cleaning agent type mild odor. Only has one bead of MS4 and a small layer of dry Potassium Carbonate in the bottle.....and I've opened it quite a bit for testing. About 1/4 has evaporated if that much. It's not the first time I've made an NAN with similar effects/odor, BUT it's certainly not often. So the goal is to find the best reproducible method - even if it means having to make less at a much slower pace - because improved results are so worth it.

I will repeat the published method again, using argon gas to see if this makes any difference.

The Professor said on Sat, 25 Jun 2022 at 22:22...

And just like always, it turned to junk a couple of days later