panziandi
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Storing the phosphorus chlorides - a bit of advice
Now I know the phosy chlorides are the sort of holy grail for some home chemists. Some of us are lucky enough to be able to purchase them, others have
to make them, still others can't do either. Sauron mentions some alternatives. Woelen has posted about ampouling sulphuryl chloride etc. I'd just like
to offer some information on my experiences with both PCl3 and PCl5.
PCl5, I had 100g in a glass bottle with PE lid with polycone insert. This was fine until I opened it, once I opened it HCl built up inside and the lid
soon degraded, the polycone had a chared appearance and the outside of the PE lid attracted droplets of water and darkened. I repacked this into two
amber glass wide-mouthed jars with teflon lined lids, this has proved very effective at storing it.
PCl3 I have stored in two modes.
Firstly I have 500mL of the chemical in a brown glass jar with a black (phenolic?) lid, this has kept the PCl3 well with no signs of leakage of either
the liquid or HCl gas! I have 100mL in a bottle which had a teflon lined lid. Now I went to wrap PVC tape around this and the lid fell apart in my
hand and i spilled some PCl3... This stuff is not nice to spill! It appears that perhaps the PCl3 leaked under the not-so-well-fitting teflon liner
and attacked the cap?
Secondly I have ampoules of PCl3 about 5mLs in each. Now these are very old likely over 20 years and are from a well known supplier. The PCl3 is in a
nice condition but I have noticed HCl attracting moisture around the box. On further investigation I noticed one had leaked to about half it's volume
and ammonia solution clouds aroun the top of the ampoule. Now there is no obvious crack or hole but clearly there is.
If you make or purchase phosy chlorides make sure you bare in mind just how much they love water and will form HCl! I strongly recommend teflon lined
caps, even though a UK supplier used a polycone insert. I also would recommend ampoules but make sure they are properly sealed and bare in mind that
if they were not sealed under inert gas that they may contain considerable pressurised HCl when you come to open them!
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Klute
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Thanks alot!
I've been pretty satisfied by keeping POCl3 in amber bottles and teflon-lined lids too, well covered by parafilm. The original container also had some
droplets near the lid once opened, under the parafilm. But i suppose POCl3 is perhasp less avid than PCln's.
\"You can battle with a demon, you can embrace a demon; what the hell can you do with a fucking spiritual computer?\"
-Alice Parr
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Picric-A
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cool thanks for the heads up!
Are the polycone things you talk about PTFE ?
Picirc-A
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panziandi
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Nopolycones are PE i think or PP, teflon liners are either white or offwhite waxy looking discs usually although they can be cone shaped too.
Polycones refer to the transparent cones under some lids like aromatherapy oil bottles. They are great for less aggressives such as acetone etc but
useless against acid chlorides etc! I also wrap PVC electrical tape around the lids. So far nothing has escaped (or entered), the PCl5 is a free
flowing powder with a few small lumps (but thats how it came as LR grade!).
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woelen
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I now have ampouled the following chemicals, in 20 ml ampoules, all wrapped in kleenex tissue and put in a bigger plastic container:
- 40 ampoules of SOCl2
- 11 ampoules of SO2Cl2
- 17 ampoules of CH3COCl
We have had a very hot period in July and all of the ampoules survived that period. I store the ampoules in another place than my lab, just too nasty
to have them inside the house.
Only one of the SOCl2 was somewhat smelly, but this already occurred the day after I made the ampoules, so I think that was a 'prodction error' and
not a problem with the ampouling method itself. This single ampoule I broke and that 20 ml now is my amount, used for experimenting.
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