Hi,
I'm doing some development work with thionyl chloride and we are getting residues in our reaction. The round bottom containing the thionyl chloride has nothing else in it, just thionyl chloride. We are keeping this inert with nitrogen which would contain trace levels of water. We are seeing a mixture of a brown, slimy material once the vessel is emptied and a fine white salt like material.
We're expecting the reaction between SOCL2 and H2O to give us HCl and SO2 and nothing else but this doesn't explain our brown slime or white salt. Any suggestions on what it is or what we've got?
Thionyl chloride (SOCl2) seemingly got contaminated with sulphur chlorides, including disulphur dichloride (S2Cl2), possibly due to its thermal decomposition.
What have you tried so far in terms of analysis? Can the powder be separated? Then you could use EDX for elemental analysis. What about IR for the slime? And does the slime form under inert conditions or when the flask is exposed to air?
Dear Philip,
Doing elemental analyses for these residues is necessary to know what other elements may be present. However, I may think about presence of some elements in water which would contain trace levels (as you mentioned) such as Fe which may formed brown, slimy material as a result of formation of Fe2S3. As well as, presence of traces of Mg( in water as trace levels) may lead to the formation of MgCl2 (will appear as white ppt.) as a direct reaction with HCl liberated from SOCl2 and water.
Best wishes
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