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Author: Subject: Purifying this store bought ammonia
sargent1015
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[*] posted on 7-10-2012 at 16:31
Purifying this store bought ammonia


Hey guys, I recently bought some shurefine ammonia, unfortunately, it says sudsy on it. But, it was cheap and I didn't really think it would be a huge problem to get out.

My test was to add some to some copper sulfate and get the complex. To my surprise, I got the dark blue complex and a light blue solid. I am thinking that the "sudsy part" is nothing more than Na2CO3 and I just made copper carbonate. This makes sense since, after I stirred the mixture, it all reacted and I lost the pretty blue.

Now, the MSDS is not online and I am waiting for an email from the producer, but does anyone have ideas on how to get rid of the "sudsy" part? I like that this product was .99 for 2 quarts, but it is ridiculous if the contaminant is what I think.

Thanks guys for the replies!




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DougTheMapper
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[*] posted on 7-10-2012 at 16:53


Heating the solution will drive off the ammonia. Bubble the gas into cold distilled water to make whatever concentration you wish.

Ammonia solubility in water:

47% (0 °C)
31% (25 °C)
28% (50 °C)

Ideally use a fritted sparging tube. Alternatively a vigorously magnetically-stirred flask of ice-cold water should do the trick for anything up to 15-ish percent.




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sargent1015
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[*] posted on 7-10-2012 at 17:11


Hmmm, I'll give it a shot!



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[*] posted on 7-10-2012 at 17:35


Depending on the concentration you need, you can also seal two beakers in a plastic bag, one with distilled water and the other with ammonia solution. Eventually they will equalize in ammonia concentration, one pure and the other with the suds in it. Keep in mind that the end result will be of a little less than half of the original concentration.

This works for pretty much all aqueous dissolved gas solutions like HCl, formaldehyde, methylamine, etc.

[Edited on 8-10-2012 by DougTheMapper]




Victor Grignard is a methylated spirit.
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sargent1015
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[*] posted on 7-10-2012 at 17:45


That sounds substantially easier (life of a college student), So I'll for sure give that a try



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[*] posted on 7-10-2012 at 18:29


I was going to say.. Doug's method is a whole lot easier to do than hunt fritted sparging tubes with 24/40 heads..believe me I've been trying for a good while now.
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[*] posted on 8-10-2012 at 00:47


It just so happend that I purified the same "sudsy" ammonia myself recently.
The way I did it was to fill a 500ml Erlenmeyer flask to around the 300ml mark with this ammonia, stopper the top and then run a hose out from that little nozzle in the side.
The hose fed through to the bottom of a very tall, very thin glass jar (the taller and thinner the better). My jar was a fancy jar for holding olive oil and it has a bottom diameter of about 45mm, a height of around 300mm and a top diameter of about 20mm. A tall measuring cylinder would work well too, though.
Anyway, the jar was filled with ice-cold water and was sitting in a bigger jar also full of cold water, with extra ice cubes :)
So what you do is heat up the sudsy ammonia until it is boiling. This drives off the ammonia because the solubility of gasses decrease as the temperature increases. The ammonia gas, along with a small amount of water is bubbled through the cold water to re-dissolve it. I dont know how concentrated the ammonia is but when I smelt it it nearly burn my nose off, so it cant be that dilute.
The solution of ammonia you get of is perfectly clear, and much purer than anything you would get via reacting all the soap away. The process isn't that efficient, but like you said the sudsy ammonia is very cheap.

Also the MSDS of "cloudy ammonia" which is the exact same stuff as "sudsy ammonia" can be found here:
http://www.cleanwithsupreme.com.au/download/Cloudy%20Ammonia...
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borrowedlawyer
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[*] posted on 8-10-2012 at 02:54


Quote: Originally posted by Oscilllator  
It just so happend that I purified the same "sudsy" ammonia myself recently.
The way I did it was to fill a 500ml Erlenmeyer flask to around the 300ml mark with this ammonia, stopper the top and then run a hose out from that little nozzle in the side.
The hose fed through to the bottom of a very tall, very thin glass jar (the taller and thinner the better). My jar was a fancy jar for holding olive oil and it has a bottom diameter of about 45mm, a height of around 300mm and a top diameter of about 20mm. A tall measuring cylinder would work well too, though.
Anyway, the jar was filled with ice-cold water and was sitting in a bigger jar also full of cold water, with extra ice cubes :)
So what you do is heat up the sudsy ammonia until it is boiling. This drives off the ammonia because the solubility of gasses decrease as the temperature increases. The ammonia gas, along with a small amount of water is bubbled through the cold water to re-dissolve it. I dont know how concentrated the ammonia is but when I smelt it it nearly burn my nose off, so it cant be that dilute.
The solution of ammonia you get of is perfectly clear, and much purer than anything you would get via reacting all the soap away. The process isn't that efficient, but like you said the sudsy ammonia is very cheap.

Also the MSDS of "cloudy ammonia" which is the exact same stuff as "sudsy ammonia" can be found here:
http://www.cleanwithsupreme.com.au/download/Cloudy%20Ammonia...


I pretty much did that exact same procedure, however I am not sure I am getting that much ammonia to go in to solution, as I forgot an ice bath. I will try and redo it after I titrate with sulfuric acid.

[Edited on 8-10-2012 by borrowedlawyer]
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[*] posted on 8-10-2012 at 21:10


Yeah the ice bath is very important, because ammonia is much more soluble at lower temperatures, and the gas being bubbled through is hot, so you'll end up heating up the water and thus getting a very weak solution.
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[*] posted on 9-10-2012 at 11:44


If the cloudy stuff was sodium carbonate, it would dissolve to give a clear solution.
I suspect it's soap.
Copper soaps are not soluble in water so you would get a blueish precipitate.
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[*] posted on 9-10-2012 at 13:55


Will copper soaps dissolve in acid? I tested this with a little HCl and it dissolved outright, didn't seem to be any evolution of gas



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[*] posted on 3-12-2012 at 19:04


Would a 100mL graduated cylinder be a good container for the resulting ammonia solution?
Also, if you use the same volume of cold, distilled water as ammonia, would you get the same concentration, within reason?




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[*] posted on 3-12-2012 at 20:08


They would equilibrate at half the initial concentration of the ammonia I believe. I wouldn't use a grad cylinder just due to the odor, unless you have some parafilm or stopper to dedicate to the task



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[*] posted on 3-12-2012 at 21:18


So, if I use half the amount of cold, distilled water, I should obtain a smaller amount of equal concentration of ammonia. No idea if that's right, but it sounds right.



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[*] posted on 3-12-2012 at 21:39


Quote: Originally posted by unionised  
If the cloudy stuff was sodium carbonate, it would dissolve to give a clear solution.
I suspect it's soap.
Copper soaps are not soluble in water so you would get a blueish precipitate.


Except they would just re-solvate as tetraamine carboxylate. Assuming it's a carboxylate "soap" and not a chelating agent or sulfonate sulfactacant...or both.




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[*] posted on 3-12-2012 at 23:14


I doubt it's a carbonate as it sounds more like a stearic acid or some other soap. Try adding Mg ions to the solution to see if the soap precipitates out.




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[*] posted on 3-1-2013 at 13:04


Any advice for bubbling a gas into water? I've had suckback problems, even with that inverted funnel trick.



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[*] posted on 3-1-2013 at 13:10


don't submerge the funnel too much.



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[*] posted on 3-1-2013 at 13:20


I have a nice gas washing bottle that I've tried to use in a very similar experiment, but I've had suckback problems with that as well. Barring the inverted funnel trick (I want to use my glassware otherwise I admit the purchase was unnecessary!), any tips on preventing suckback in such a setup?

My ammonia gas generator was an RBF that led to a vacuum takeoff adapter and a smaller RBF (to catch suckback), and the takeoff was led to the input of the gas bottle. Pretty much as soon as ammonia started to evolve there was immediate suckback to fill the little RBF. :mad:
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[*] posted on 3-1-2013 at 13:25


Trying to visualize your setup... failing miserably.
I think suckback has to do with the bubbler itself, it creates a vacuum thus sucking up the water and such. Which is why glass fritted disks are apparently gold in this situation.
Anyway, what about concentration by freezing, analogous to hydrogen peroxide?




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[*] posted on 3-1-2013 at 13:48


This is the gas wash bottle I'm talking about :


The gas goes in the inlet on the left and bubbles up through the glass frit at the bottom. The idea was to pass in ammonia gas and dissolve it in the water in this bottle. The gas was generated in a ground-glass type setup that had a large RBF as the reaction flask, with a smaller RBF in between that and the wash bottle to catch potential suckback. The whole system was ground glass, and so was sealed up until the outlet of the wash bottle which was open to the atmosphere. Hope that makes a little more sense.
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[*] posted on 3-1-2013 at 13:55


Damn, I wish I had one of those! Where did you obtain yours?



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[*] posted on 3-1-2013 at 14:00


http://www.hinmeijer.nl/product/46938/Gaswasflessen.aspx
there you go




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[*] posted on 3-1-2013 at 16:08


This is my setup, it's not perfect but it seems to work.



Normally the funnel would be inverted into a beaker, but you get the idea.




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[*] posted on 4-1-2013 at 06:26


Hexavalent, I got that bottle from good old Dr. Bob. I think it was one of his last ones, but it'd be worth a try to ask him if he has more!
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