Italian method for making nitrites

Topic created by Nitritespecialist
on Thu, 7 Oct 2021 at 14:23

Nitritespecialist said on Thu, 7 Oct 2021 at 14:23...

An amount of 1 mL ofthe suitable alcohol was added to a mixture of 0.2 mL water and
1 mL concentrated sulfuric acid (96%) ~n a 50 mL flask chilled in an ice bath, under nitrogen
atmosphere in the dark. The mixture 'fas shaken for 10 min, then an equimolar solution of
sodium nitrite (4 mL) was added dropwise with periodic shaking. The solution was shaken
at five minute intervals for an hour.ithen let stand to permit the separation of the alkyl
nitrite from the aqueous layer. The upper alkyl nitrite layer was mixed with anhydrous
sodium sulfate, then transferred into a small vial and sealed

Nitritespecialist said on Thu, 7 Oct 2021 at 14:29...

The above synthesis was done in the late 90's to determine what's in street poppers and how exposure to sunlight degrades them. They made all the common nitrites in their lab and tested 0.2 ml of them immediately after making them. Only the street samples and their in house samples that had been exposed to 2 hours of sunlight had a bunch of different impurities...at least 3 of which were "acids".

Notice how much time it took for them to make roughly 1 ml of nitrite. It took over an hour and they used 1 ml of conc. sulfuric per 1 ml alcohol. That's a lot. They used 4 mls of SN solution....presumably that's about 0.7 grams of SN in 3.3 mls of water, which is less than a 25% concentration.

Nitritespecialist said on Thu, 7 Oct 2021 at 14:31...

They performed the reaction under nitrogen and in the dark as well...using cold temps.

Perhaps the cold temps slow down the reaction so much that ample time is needed to make certain the reaction is complete. No explanation was given.

The Professor said on Thu, 7 Oct 2021 at 17:11...

The samples were prepared with the intention of studying photochemical degradation and decomposition of alkyl nitrites. Looking at the graphs for the reference standard sample, they obtained an extremely pure nitrite in doing it that way.

The Professor said on Thu, 7 Oct 2021 at 17:18...

there's a lot of priceless data in that writeup; the fragmentation patterns will tell you about possible cation/anion recombinations, which you can then compare with activation energies and design an apparatus that eliminates the possibility of degradation components during synthesis.

In combination with the other writeup on HOW the nitrite decomposes/degrades one can also design a suitable storage environment that prolongs the viability of the nitrite.

together, those two writeups contain most of the answers a maker might be seeking

Nitritespecialist said on Fri, 8 Oct 2021 at 19:12...

I tried this method to make IPN today - about 5 mls. I didn't follow exactly, but as much as I could. I used 91% IPA and battery acid, low 30s in percent sulfuric. And I didn't have nitrogen gas...but I kept covered in the dark...very slow stir on ice. I used food grade SN.

It seemed to work. Got a yellow sweet, highly volatile IPN, but as usual - terrible side effects right away in less than 5 minutes.

Didn't get any sulfate precip.

6.5 mls IPA. 18 mls battery acid(about 6 mls acid, 12 mls water) and 4.2 grams SN into 18mls water.

There was quite a bit extra water, so not sure how that impacted the reaction.

I'll try later with amyl/butyl/conc. acid when I order more.

Wenis said on Sun, 25 Dec 2022 at 06:29...

Hey jessie hey whalter ;-)