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Author: Subject: Obtain Nitrosyl Tetrafluroborate
APO
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[*] posted on 15-5-2013 at 00:48


I read that he thinks his had some WP contamination, but I got mine from matchboxes, so... Should I just buy Phosphorus Trichloride from Sigma Aldrich?



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[*] posted on 15-5-2013 at 00:54


Quote: Originally posted by APO  
I read that he thinks his had some WP contamination, but I got mine from matchboxes, so... Should I just buy Phosphorus Trichloride from Sigma Aldrich?


You can't buy anything from Sigma Aldrich - though I'm sure the person on the other end of the phone would get a kick out of you trying. You (specifically) really can't buy chemicals from anyone other than people on Amazon or Ebay (online). Any actual chemical supplier such as Sigma Aldrich require a commercial address, and will give you a 'shit test' over the phone. I.E they will ask what your company does, what the chemicals are for ect.. At least until you have an account established with them.

Though you could probably get away with buying from pyrotechnic stores online - to my knowledge many of them require the signature of someone +18 upon delivery.
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What a scary world it would be if anyone of any age could purchase chemicals from Sigma hahaha.

[Edited on 15-5-2013 by Hockeydemon]
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[*] posted on 15-5-2013 at 22:54


Burn phosphorus in a chlorine atmosphere and condense the vapor.
Can be done easily in a flask. Purge a flask with Cl and add P and heat.
The flask will get coated with PCl3.




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[*] posted on 16-5-2013 at 03:38


No, this does not work. You'll get mainly PCl5. Besides that, isolating the material from such a flask with a thin layer sticking to the glass is nearly impossible. PCl3 and PCl5 are extremely moisture sensitive and even simply opening and closing the flask will spoil your product. Remember you have a thin layer on the glass and all of it will come in contact with (humid) air.

You need a LOT of chlorine for a little phosphorus. You really need to make a chlorine gas generator, dry the gas perfectly well and have to lead the gas over phosphorus. The reaction is extremely violent, so the phosphorus must be suspended in some inert solvent. Your biggest enemy again is formation of PCl5, which clogs tubes and may lead to severe high pressure failures of the gas generator!

This really is not something for beginners! If I were father of a teenage boy then I never would allow him to do this kind of experiments, certainly not in an apartment.

I have some PCl5 and I have some PCl3 and both chemicals are truly nasty to work with. The bottles of these chemicals are pressurized with HCl and both chemicals give off intensely choking fumes and every metal object nearby corrodes like hell. I made some PCl5 into a glass ampoule and I have a 25 ml commercial ampoule of PCl3. Nice to have as samples or curiousities, but hardly useful for experimenting in a home setting, unless you have a really good fumehood, which has a motor and suction system which is corrosion resistant. This is how these chemicals look like (both are my samples in glass ampoules).

http://en.wikipedia.org/wiki/File:Phosphorus_trichloride_25m...
http://en.wikipedia.org/wiki/File:Phosphorus_pentachloride_a...


[Edited on 16-5-13 by woelen]




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[*] posted on 16-5-2013 at 03:57


Sorry to get off-topic (this thread still had a topic?) but how do you fix that? The unintentional smilies.



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[*] posted on 16-5-2013 at 04:47


Quote: Originally posted by Finnnicus  
Sorry to get off-topic (this thread still had a topic?) but how do you fix that? The unintentional smilies.


The checkbox 'disable smilies' :) :P :D
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[*] posted on 16-5-2013 at 12:49


I could use Disulfur Dichloride instead, would that be easier to obtain/make or be safer to work with?



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[*] posted on 16-5-2013 at 13:02


I disabled the smileys and now the links work.



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[*] posted on 16-5-2013 at 13:16


Quote: Originally posted by APO  
I could use Disulfur Dichloride instead, would that be easier to obtain/make or be safer to work with?


Wrong. You must study chemistry better. You may use PCl3, POCl3, SO2Cl2 (but no S2Cl2!). All these stuffs are not for beginners. There is a way to prepare Ac2O without such compounds. But if you do not want to start with something simple, you'll definitely fail.




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[*] posted on 16-5-2013 at 14:00


Ac2O being Acetic Anhydride? Also I'm just planning right now, I'll definitely wait till I get better equipment. I'm just trying to know easier/safer ways to make Acetic Anhydride. Or, if there's a place where I can buy it without being put on a watch list, that's fine too.



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[*] posted on 17-5-2013 at 02:06


I can enlighten you, if you do not know- Ac2O is used to make heroin from morphine. This is why this compound is under control. Make picric acid- it gives you both detonator (0.5 gr of its lead salt + 2 gr of pressed picric acid) and main charge-same picric acid or its ammonium salt mixed with AN. Kalium salt is interesting compound too- it burns quickly on open air and blow up, been ignited in confinement. And it is not as sensitive as usual primaries like TATP or MF.



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[*] posted on 17-5-2013 at 14:19


I can buy Picric Acid from HMS Beagle?

http://stores.intuitwebsites.com/beaglewebstore/-strse-1446/...




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[*] posted on 17-5-2013 at 14:49


I saw that a long time ago, it has been out of stock for about a year. Also seems pretty expensive when you can make a lot more in a day from a $5 bottle of 300 aspirin and about $10 worth of acid.



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[*] posted on 17-5-2013 at 15:13


Just wondering if anyone has bought some.



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[*] posted on 17-5-2013 at 22:09


In my youth I saw picramic acid in a specialized shop, where I bought phenol, toluene and so on. They did not sell sulfur acid (to say nothing about nitric one) without corresponding papers (it means, not for private person). Sulfur acid of 92-94% could be bought just across the street. But preparation of picric acid is simple- look for a corresponding tread. I think, that phenol a a precursor is better than ASA, if you only can get it.



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