Sciencemadness Discussion Board

Yellow residue in ammonia solution

nezza - 23-1-2016 at 12:05

I recently bought a couple of hundred ml of "pure" ammonia from a chemical supplier. It is stated to be 28% or so. It arrived in a dark plastic bottle and after a few days storage in a fridge there is a pale yellow solid at the bottom of the bottle. I originally thought it might be ammonium carbonate/carbamate but it does not appear to be.

I have filtered it out and the solid appears to be some sort of organic.
It burns with a smoky flame leaving no residue.
It does not dissolve in dilute acid.

Does anyone have any idea what it might be ?.



hissingnoise - 23-1-2016 at 13:07

Quote:
Does anyone have any idea what it might be?

An aromatic amine, from contaminated hydrocarbon feed gas, would be my guess!


nezza - 24-1-2016 at 02:45

Thanks for the suggestion hissingnoise. I have tried diazotising and coupling it to thymol. No colour reaction so I don't think it is a primary aromatic amine.

I think I'll start from the top and do a sodium fusion test to see if it contains nitrogen, halogen or sulphur.

[Edited on 24-1-2016 by nezza]

hissingnoise - 24-1-2016 at 07:02

Leaving the soln. in a freezer overnight should precipitate the impurity, leaving it clean enough for most!

If you want pure NH4OH you'll have to distil . . .


nezza - 24-1-2016 at 08:12

Thanks again. I'm just interested in what the inpurity is.

I've had another look at the impurity.
The solid does NOT contain any occluded ammonia (negative with Nesslers).
It melts to a pale yellow liquid and boils with some decomposition (Ammonia smell).
It is insoluble in alcohol, water and toluene.
It does not contain sulphur or halogen but does contain nitrogen.
It does not react appreciably with bromine water (not unsaturated).
The solid appears as pale yellow optically active monoclinic crystals.

Crystals.jpg - 63kB

hissingnoise - 24-1-2016 at 08:43

Quote:
I'm just interested in what the impurity is.

Wow! That all-too-rare pioneering instinct?