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sargent1015
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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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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.
Victor Grignard is a methylated spirit.
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sargent1015
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Hmmm, I'll give it a shot!
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DougTheMapper
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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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That sounds substantially easier (life of a college student), So I'll for sure give that a try
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Funkerman23
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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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Oscilllator
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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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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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Oscilllator
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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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unionised
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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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sargent1015
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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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elementcollector1
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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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sargent1015
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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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elementcollector1
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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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UnintentionalChaos
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| 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.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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Sedit
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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.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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elementcollector1
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Any advice for bubbling a gas into water? I've had suckback problems, even with that inverted funnel trick.
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Pyro
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don't submerge the funnel too much.
all above information is intellectual property of Pyro.  |
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MrHomeScientist
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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. 
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elementcollector1
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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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MrHomeScientist
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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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Hexavalent
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Damn, I wish I had one of those! Where did you obtain yours?
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
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Pyro
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http://www.hinmeijer.nl/product/46938/Gaswasflessen.aspx
there you go
all above information is intellectual property of Pyro. |
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elementcollector1
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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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MrHomeScientist
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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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