03-04-03 04:52
No 413538
Just a quick question. In the hydrolysis of amyl alcohol, would calcium hydroxide be a suitable substitute for lye? If yes, any pointers (longer/hotter reaction, etc)? Much appreciated.
[Edit] Err, the hydrolisis of amyl acetate TO amyl alcohol. Sorry. >_<
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Chief Bee)
03-04-03 05:23
No 413544
It would not be as good, due to its low solubility. Neither Ca(OH)2 nor Ca(OAc)2 is very soluble, and as Ca(OH)2 is not as strong a base as NaOH, the reaction would also go slower. Why don't you want to use NaOH?
(Hive Bee)
03-04-03 06:02
No 413553
Ok, point well taken regarding thier solubilities. I had already figured the reaction would take longer, for the same reason you stated.
My only qualm with using NaOH is that my only current source is Burgandy Demon Lye. I have heard many times that the stuff is impure. On the other hand, Calcium Hydroxide is very easy to get in large quantaties relatively pure.
Oh well, looks like the Demon Lye will get a shot at it, especially since the amyl alcohol will probably be distilled.
Thanks for the info Rhodium.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Old P2P Cook)
03-04-03 06:24
No 413556
I have heard many times that the stuff is impure.
AFAIK, this is nothing but a spurious excuse that has been used on occaision by tweakers to explain a failed batch.
All those moments will be lost in time, like tears in rain.
(Hive Bee)
03-04-03 06:41
No 413557
I have never really been sure one way or the other on the issue. Thanks for the enlightenment terb. SWID shall press onwards, with the burgandy demon by his side.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Hive Bee)
03-06-03 00:12
No 414119
In an old post ( Post 236493 (Aurelius: "Re: Nitrite from Nitrate, using Fe", Chemistry Discourse)), I found the equation 2NaNO3 + Ca(OH)2 + C --> 2NaNO2 + CaCO3 + H2O. Is there any reason to think this wouldnt work equally well for potassium nitrate?
[Edit] Oh, and one more thing...in the patent report it states that graphite is the best form of carbon to use. What about the activated carbon that is commonly available at aquarium supply stores? I am unclear on the difference between activated and unactivated carbon...
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Chief Bee)
03-06-03 01:47
No 414124
Graphite is crystalline carbon in sheets, and activated carbon is amorphous and porous.
(Hive Bee)
03-06-03 03:30
No 414156
Oh. That sounds like another case of ancient colloquial alchemist nomenclature which needs to be updated. Oh well.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Hive Bee)
03-09-03 05:51
No 414949
Quick question, does anyone know the solubility of sodium nitrite in isopropanol? I am asking because the Merck 12th doesnt list it. It is needed to try and devise a method for seperating sodium nitrite from sodium chloride. Any help would be much appreciated.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Chief Bee)
03-09-03 19:28
No 415065
http://www.ussaltllc.com/Specifications/
(Hive Bee)
03-09-03 20:06
No 415082
Thanks Rhodium for the link
, but there were several pictures on that page which would not load...and those were the pictures with the solubility data tables. 
No biggie, I will do some searching myself. I was just hoping that someone had already devised a method.Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Master Searcher)
03-09-03 21:29
No 415105
This is worth looking at.
http://www.geocities.com/dritte123/NaNO2
Did this disappear? Post 9162 (not existing)
Post 235961 (otto: "Re: Nitrite from Nitrate, using Fe", Chemistry Discourse)
http://www.geocities.com/dritte123/PSPF.
The hardest thing to explain is the obvious
(Hive Bee)
03-11-03 01:37
No 415511
HCl + NaNO2 -> NaCl + HNO2 ???
Does this reaction occur when HCl is added to Sodium Nitrite? Also, does sodium nitrite's solubility decrease in muraitic the same way sodium chloride's does? All these questions are obviously in relation to the separation of the chloride from the nitrite. Any help is appreciated, as data regarding NaNO2 seems suprisingly sparse. Again, many thanks.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Hive Bee)
03-11-03 16:06
No 415712
Nevermind, I am being an idiot.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Hive Bee)
03-11-03 18:14
No 415752
Is there any reason to think that HCl would not work in the synthesis of amyl nitrite, assuming of course equimolar amounts compared to the standard addition of sulfuric. Is chlorination of the alcohol possible, resulting in some nasty 'chlorinated solvents'? Also, would sodium chloride in the reaction cause problems? Here is the current thought:
NaCl + NaNO2 + Amyl Alcohol + HCl -> NaCl + Amyl Nitrite + H20
Anyone take issue with this? Tests will be performed, results posted...eventually.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
(Hive Bee)
03-11-03 19:59
No 415784
NaNO2 + HCl --> NaCl + HNO2
HNO2 + C5H11OH --> H20 + C5H11ONO
And yes, concentrated HCl works for the synthesis of amyl nitrite, you should expect about 70-80 % yield of amyl nitrite.
Quidquid agis, prudenter agas et respice finem!
(Hive Bee)
03-13-03 00:38
No 416296
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 H2SO4 * 18.4mol H2SO4/L * 1mol Hcl/ 1mol H2SO4 * 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.
Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^