Author Topic: Glacial Acetic Acid - Help Please Urgent( to me)  (Read 528 times)

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Propoxyfiend

  • Guest
Glacial Acetic Acid - Help Please Urgent( to me)
« on: February 18, 2003, 01:49:00 PM »
Most likely swim has no business in a lab.  Swim accidently spilt their bottle of GAA.  Swim is in desperate need of some GAA.  The search engine was searched.  Some 60 + posts were found which are being reviewed now.

Not in my part of the country (mid-south USA). SWIM EVERY fuckin photo-related store that was in the yellow pages and not even one carried it (most didn't even know what it was). SWIM ended up having to go through local chem supplier.


Swim is having the problem as this fellow.  Swim has even checked major surrounding cities, no luck.  Should swim call it a different name?  Swim has heard it can be distilled from
White Vinegar. Is this an upto date and acceptable method:


Materials:
Gallon of White Vinegar.  (Try to get 9% acidity "pickling" vinegar)
Container of Lye Anyone have any idea how much total
Sulfuric Drain Opener
pH paper
Distillation rig
Plastic bucket
Large cassarole pan(sp?)  Pyrex glass and Corning ceremics are good.

Method:
Pour vinegar into the bucket.  Add lye a little at a time.  Bee careful about that volcano action.  Also always keep lye bottle closed when not using it.  And don't use a metal spoon.

Sodium Acetate is being formed.  It is water soluable so you won't see it.  Keep adding lye until it stops fizzing when more is added.  Check the pH.  You are shooting for a pH between 7 and 9.  If it is below 7 then, when you go to concentrate it, some of the vinegar will vaporize and stink.  The higher it is above 7 the more unreacted lye will be left over so add slowly.

Pour the liquid into your cassarole dish.  The inevitable extra lye is why you've gotta use glass.  Lye will react with the glass but very slowly.  Whatever you do don't use an aluminum pot!  Put it in the oven at 300C so that the water will all evaporate away.  Expect it to take many many hours. anyone know how long many many translates to?

When all the water is gone you'll be left with a crusty substance that is mostly sodium acetate but also probably a little bit of lye.  You will be happy if you are not using a white cassarole because it will be easier to see it and get it all out when you start scraping...

Slowly and Carefully add sulfuric drain opener.  Distill and collect between 110-125.



If anyone has a better method or suggestions feel free to advise.

Thanks for the help!  In advance!
 

 




sean1234

  • Guest
i suggest going into a photo store and looking
« Reply #1 on: February 18, 2003, 02:15:00 PM »
i suggest going into a photo store and looking at labels. they WILL have glacial acetic acid.
i was just in a local photo shop in a fairly small town and there was tons of GAA!

thallium

  • Guest
Google...
« Reply #2 on: February 18, 2003, 02:29:00 PM »
A simple search on Google shows a bunch of pages with brand names and suppliers... It would definitively be much easier for you to order it instead of producing it ourself.

Loking at the links I can see that GAA is used for stop baths; I am sure your local photo supply will help you further :)  Good luck!

http://www.google.com/search?sourceid=navclient&q=acetic+acid+photo




Propoxyfiend

  • Guest
Ugh - Thanks for the help?
« Reply #3 on: February 19, 2003, 07:54:00 AM »

A simple search on Google shows a bunch of pages with brand names and suppliers...  I am sure your local photo supply will help you further  :)   Good luck!


  I am happy people sell GAA.  Truthfully, this is no shocker to me. I am glad people sell it in your area as well.  I am certian this makes it much easier for you to obtain.  Swim would love to walk into a store and purchase some GAA, this would be too cool!  However, after serious consideration and deep thought swim's decided not to move closer to where you live.  Swim fully understands if they moved to your area they could purchase GAA with ease, like you(lucky bastard)  But, this is not an option(today). . .   Swim has already called all the local suppliers in their town.  It's just not carried.  If the TFSE is checked on The Hive you will notice other people saying it's not available in their town either.  Swims problem is the location of their equipment will only be vacant for 1-3 more days.  Overnight shipping would more than double the cost of this stuff.  If it's as easy to make as my earlier post said swim doesn't think it seems smart to tax on another $20 shipping fee. Anyhow, if someone could help with the original 2 questions(1st post) and. . . In reference to the first post there is one last question


Slowly and Carefully add sulfuric drain opener.  Distill and collect between 10-125.


How much sulfuric acid is added? 

Note about the "Google Crack" over 1080 hits were found on google alone not to mention: About, Ask, Yahoo, Dogpile, Excite and others.  Swim is well aware of how to use a search engine, I think?  But, swim doesn't have time to read all 1080"
Swim doesn't mind spending countless hours reading, researching and learning but feels this is unnecessary.




thallium

  • Guest
OK... Here you go :-) One gallon of 9% acetic...
« Reply #4 on: February 19, 2003, 10:18:00 AM »
OK... Here you go :)

One gallon of 9% acetic acid (try to get 35%) = 3.8L = 3800g

3800g x 9% = 342g CH3COOH.

342g / 60.05g/mol = 5.7mol CH3COOH

6mol NaOH = 6mol x 40g/mol = 240g NaOH

You require at least 240g NaOH

You would need about 7mol H2SO4 = 7mol x 98.08g/mol = 687g pure H2SO4

Don't know what strenght drain opener you have avaliable; so you'll have to do the rest of the math yourself :)


Expect it to take many many hours. anyone know how long many many translates to?




3-4 hours...?

(Hope I did the math correctly; didn't have my Merck avaliable, so I had to look up the mol weights on the net. :) )

Edited wrong gallon size; thank you psytech :)




Chromic

  • Guest
Answer
« Reply #5 on: February 19, 2003, 11:43:00 AM »
I've done this conversion before. I would recommend that you distill your vinegar if you want to make pure sodium acetate. I think all that is commercially done to clean up vinegar is a microfiltration or centrifugation to make it look clear. (but it's not pure or anything)

I'd add baking soda until the dilute acetic acid stops fizzing. Then add about 5% extra dilute acetic acid (or, 5% after the bubbling stops--IIRC, it's something like just under 70g of NaHCO3 for each liter of distilled vinegar). Boil it off, there should be a light (not heavy) smell of vinegar as it boils down. That's your sodium acetate. If you distill the vinegar, it will be white. If not, it will be a gross brownish-black color. Make sure it's good and dry before going on to the next step.

In a 500ml flask add 150g NaOAc, then with good cooling, VERY SLOWLY, VERY, VERY SLOWLY add 270g H2SO4. (you need a large excess of sulfuric acid)

You should be able to to distill off about 85g acetic acid (about 80% yield) before your flask will fill with foam. Collect 110-120C.

sean1234

  • Guest
. Swim has already called all the local ...
« Reply #6 on: February 19, 2003, 02:50:00 PM »
.   Swim has already called all the local suppliers in their town.  It's just not carried. 

I no photographer but from the looks of the products that i saw in my local photo shop when I WALKED IN AND LOOKED AROUND, i might venture to say that glacial acetic acid is fairly essential in photography. However this doesnt mean that the person behind the phone knows the chemical name of the stuff thats in thier shop. take another look in person and then you can tell us that you cant find any.

psytech

  • Guest
wrong
« Reply #7 on: February 19, 2003, 04:57:00 PM »
One gallon of 9% acetic acid (try to get 35%) = 4.6L = 4600g
on us gallon is = to 3.7854344965615545 liters