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RogueRose
International Hazard
Posts: 1593
Registered: 16-6-2014
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So I have an update on the ammonia sulfate solution that I mixed with Ca(OH)2. As I noted before I made a saturated solution of 710g amm sulf &
444g of hydroxide (about 10% excess of hydroxide - I'm wondering if this may have caused a problem...) in ~1100ml water. Upon heating in an oil bath
gas stopped coming over very early and I eventually was getting ammonia solution coming over at a full boil at 100C. The boil was so intense the
flask almost filled to top before I removed from heat. So there is no question that it didn't get to boiling point.
I filtered the solution and am heating it again in oil bath and NH3 started coming over at slight heat maybe 110F and has been coming over for 20+
mins at a very "nice" rate. Very little smell of ammonia coming out of the top of the graduated cylinder that is catching the ammonia gas.
I plan to capture all the gas until it reaches the point where liquid is coming over and then I will distill over all the liquid unless it is clear
that the liquid coming over is pure water at which case it seems that all the NH3 will have been boiled out of the flask, which is what I had
originally how I expected this reaction to work.
So it seems that the CaSO4 was interfering with the release of the NH3 in the first few attempts to distill off the gas. I've kept the sulfate sludge
and it has a very strong smell of ammonia and I'm wondering what to do with it. I have considered washing it with cold water then filtering again or
I could place it in a flask and heat to release the ammonia. I may try heat a small amount to test and see if gas comes over or it the sulfate locks
it up somehow. I'm a little worried about heating the sulfate in a flask and not being able to clean it out afterwards.
I have tested using an old 400w high pressure sodium light as a boiling flask and it worked very well. It is about as thick as cheap boro glass
flasks and it could be considered disposable if it is too difficult to clean out. The bulb holds just under 1500ml. There are a number of sizes of
this type of bulb from the larger 1000w & 1500w which look to be about 4-6L and 10-14L respectively. They also have smaller ones which look just
as useful. I was heating my urea with a propane blow torch, with direct hot heat in a small localized area and it held up perfectly, so that is good
news, but I digress.
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Ubya
International Hazard
Posts: 1247
Registered: 23-11-2017
Location: Rome-Italy
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Mood: I'm a maddo scientisto!!!
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maybe CaSO4 crystals adsorbed NH3 in their structure as they precipitated
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feel free to correct my grammar, or any mistakes i make
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RogueRose
International Hazard
Posts: 1593
Registered: 16-6-2014
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Well I've found that the Ca(OH)2 isn't so pure and has absorbed some CO2. IDK if that made a difference as I added excess hydroxide.
I did take video of the process and found some interesting reactions of how the vapors are traveling. I also may have had a clogged air stone which
may have been intermittant. I had the stopper blow off my flask and was lucky enough to catch it on video..
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