Ok, here is a story dreamed up by SWID whom I spoke to telepathically in a meditation-induced trance.
1.66lbs of 6.25% NaNO2 (remaining % mostly NaCl, with a little red #5) = 47g NaNO2
41.5mL Isopropyl (give or take 5mL)
82.5mL HCl (which SWID will explain as possibly wrong in a second)
Math for acid conversion: .03589L H
2SO
4 * 18.4mol H
2SO
4/L * 1mol Hcl/ 1mol H
2SO
4 * L/4mol HCl = 165mL
This is assuming conc. sulfuric from original equation as stated, and muriatic acid for HCl source. However, SWID totally spaced taking into account that sulfuric acid has two acid groups, and HCl only one.
The numbers are different from the source document, as SWID's anonymous friend was doing a half-batch. The ratios should be correct, however.
The story goes like this: 1.66lbs of 6.25% NaNO2 was charged into a quart reaction vessel (mason jar). This was wetted with 41.5mL of Isopropanol and 100mL of dH2O. Mechanical overhead stirring with a titanium rod was used (stirred the shit out of it with a piece of scrap metal), until the salt was slightly less "cakey". The 82.5 mL of HCl was added to a volumetric flask, which was then flooded with dH20 up to 200mL. Both solutions were placed in a freezer for ~20min until cold, then removed. With the vigorous stirring in place, the diluted HCl was added to the reaction vessel in 10-25mL increments over the space of ~5 minutes. Care was taken to insure that most of the HNO2 stayed in aqueous solution by not adding the acid too quickly. The red#5 acted as a convienent indicator of remaining HCl (acidicity or side reaction?), as the red color of the solution would disappear and turn yellow-brown until the HNO2 had reacted with the isopropanol, at which point the red came back. After the reaction was complete the stirring was slowed to a gentle swirl to help bring up any isopropyl nitrite trapped in the sodium chloride at the bottom of the reaction vessel. After the vessel was left to set a minute, the isopropyl nitrite which had seperated to the top as a dirty yellow oil was syphoned off with a syringe. At this point there was >50mL of 'product'. This product was quite dirty however, and after being subjected to two sodium bicarbonate/dH20 washes to neutralize any remaining acid, the yield was only ~25mL.
Bioassay by the person who told SWID this story and some interested and expierenced 3rd parties revealed clean, pure, isopropyl nitrite.
Some side notes that were mentioned to SWID: HCl is much preferred over sulfuric, since it does not react exothermically with water. The entire reaction ran ice cold and did not need extra cooling (ie icebaths, etc.). The red #5 was actually an advantage as indicated, and when the impure product was subjected to the bicarbonate washes, the yellow oil cleared as the dH20 turned pinkish/red. The sodium chloride was also turned to an advantage when using HCl, as the NaCl pushed the isopropanol out of solution while the HCl pushed the NaCl out of solution. Wait, is that an advantage?
Last, the yield may have been increased with the addition of more acid.
The End.
Crazy story huh? Here I am wasting my time trying to make sodium nitrite, and SWID knew some dude who has the bizalls to just go out and buy the shit! Bastard.
