Just neutralize vinegar (usually 19-24%) with 25% sodium hydroxide (lye) solution and evaporate the excess water until the sodium acetate trihydrate crystallizes. A much better way of making the salt anhydrous is to nuke it in a pyrex pan in the microwave until no more water vapor is given off and the large translucent trihydrate crystals has been converted into a dry amorphous powder.
http://rhodium.lycaeum.org (http://rhodium.lycaeum.org)
vinegar (usually 19-24%)
Wow! Remind me never to put straight vinegar on my salad in what ever country you live in. Vinegar around where I live is 5% acetic acid.
I have some sodium acetate that was laborously made by neutralizing distilled vinegar with baking soda so that's no trouble there (using a small excess of acetic acid, boiling down and drying). Can you suggest how much conc sulfuric acid should be added per gram of sodium acetate? Are we talking a small excess of sulfuric acid or a healthy excess?
I do wish to appologize about pulling up so many threads from across the board. I was pissed off that there wasn't good information in any of them and thus made sure to contibute information to each thread. I'm glad they're all referencing this post where hopefully I'll give some detailed instructions.
Organikum, thank you for some of the details, I will try a freeze separation as well. I hope it will give GAA, but for some reason, I highly doubt it. Any time I've tried to freeze purify alcohol from water, it's never worked very well... I don't see why this would be any different, the acetic acid is going to be highly hydrogen bonded. Mind you... I have to say that freeze purifying anethole and safrole works spendidly!
in Post 382036 (https://www.thevespiary.org/talk/index.php?topic=6048.msg38203600#msg38203600)
(Organikum: "distilling, than freezing out", Chemicals & Equipment) you say to distill to 95% then freeze out the rest of the water. Well, the trouble is, in Post 382006 (https://www.thevespiary.org/talk/index.php?topic=6048.msg38200600#msg38200600)
(Chromic: "Drying acetic acid", Chemicals & Equipment), I show how you need a huge amount of theoretical places to be able to purify the acetic acid.
As I said, I used a 500mm fractionating column going as slowly as possible and got piss-poor results. I'm sure if I had a 50m column I could do this, but I have't yet turned my house into a chemical plant. It appears that you can't distill a substancial amount of acetic acid to a decent purity, ie 90+%.
I will try the freezing method though, can't hurt to give it a shot. I'd also love to hear how little H2SO4 I can get away with using to distill GAA from the mix. I know 59.7g H2SO4 per 100g NaOAc is what theory says, but because 86.6g of Na2SO4 would be produced, it appears that without a doubt you'd have to use more H2SO4.