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itchyfruit
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carbon disulfide
Can anyone recommend a UK supplier for carbon disulphide?
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panziandi
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Personally I recommend Fluka, that is the manufacturer of mine, but they will not even consider supplying this chemical to a private individual! You
will have to make it I expect unless anyone has some spare! There are several posts on the matter, do a forum search for "Sauron" who authored most of
the discussion on this topic.
Why on earth would you want this though? It has limited use as a solvent, often "nicer" solvents are around, limited use as a reagent. Incredibly
volatile, INCREDIBLY flammable (I kid you not, autoignites at 90*C... so it can inflame from a hot water bath!) and smells pretty foul unless its
REALLY pure, and is pretty neurotoxic (causes/exaggerates bipolar disorder).
Not trying to discourage anyone it is a delightful sight to see a bottle of it in a flammables cupboard!
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Ozonelabs
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We have some that is available- if you mail mike.ozonelabs@googlemail.com with what you want, how much of it, intended use and your age- he'll get
back to you.
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entropy51
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Itchy, I second panziandi's question about why on earth? Bungee jumping would be more fun and less dangerous. The last we heard your hood was not
safe for this stuff. The scariest thing I've ever done is to pour a few liters of CS2 out of a 5 gallon drum. I break out in a cold sweat
remembering it.
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UnintentionalChaos
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So, I've read references that say pyrolysis of metal thiocyanates gives CS2. I also know that this was brought up in another thread, and that there's
a route via tube-furnace in prepublication, but does anyone know about yields from thiocyanates? If you only need 2 digits worth of millilitersl for
something, that may be the way to go.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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panziandi
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Without checking, thermal decomposition of lead thiocyanate rings a bell, but I am not 100%. It could be done safely if the apparatus was first
flushed with CO2 to displace oxygen. Probably the way to go for 25-50mL batches at a time.
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itchyfruit
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I just wanted some for doing woelens tin iodate synthesis and for dissolving phosphorous in.
I did read the MSDS on it and i can see that transportation could be an issue especially via motorcycle 
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UnintentionalChaos
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Quote: Originally posted by panziandi  | | Without checking, thermal decomposition of lead thiocyanate rings a bell, but I am not 100%. It could be done safely if the apparatus was first
flushed with CO2 to displace oxygen. Probably the way to go for 25-50mL batches at a time. |
Give me a month and I'll have some Pb(SCN)2 to try it out with. Also check out Letts Nitrile Synthesis. The modified procedure gives good yields from
benzoic acids using the zinc benzoate and lead thiocyanate. It works moderately well for certain aliphatic systems (and not at all for others), often
with contamination by amides though.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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woelen
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| Quote: Originally posted by itchyfruit | I just wanted some for doing woelens tin iodate synthesis and for dissolving phosphorous in.
I did read the MSDS on it and i can see that transportation could be an issue especially via motorcycle |
As I have written, the reaction can also be done with CH2Cl2, which is much easier to obtain for most of us. I was pleasantly surprised by how well it
works with CH2Cl2, I expected more trouble. The only thing is that you need a little more of the solvent, but CH2Cl2 is cheap and that is not a real
issue.
Btw, I did not make tin iodate, but tin(IV) iodide 
[Edited on 19-9-09 by woelen]
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Polverone
Now celebrating 21 years of madness
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Thread Split
19-9-2009 at 09:11 |
itchyfruit
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I don't have any of that either, i do have some paint stripper that contains it but i'm not sure how to purify it,and my fume cupboard is not really
suitable for flammable solvents.
I have quite a lot of other organic solvents so i might do a few small scale tests to see which ones dissolve iodine unless someone who has seen my
list could suggest one of that will and save me the hassle
sorry iodide
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itchyfruit
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What does 'thread split' mean ?
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UnintentionalChaos
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It means the off-topic crud was split off and made into a seperate thread...in this case, moved directly to detritus.
I have some perchloroethylene...and iodine, and tin. I could give this a try.
[Edited on 9-19-09 by UnintentionalChaos]
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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itchyfruit
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I don't think i have any of that either,but i'm sure i could get some fairly easy.
Whats the solvent used i'n tinture of iodine,i may try that!!let us know how you get on !!!
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Ozonelabs
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Iodine tincture, I believe is KI/I2 in EtOH/H2O...
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woelen
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Ticture of iodine does not work, it contains alcohol and that reacts with SnI4.
I'm quite sure that perchloroethylene will work, I expect that any solvent, which does not react with SnI4 will do as long as both SnI4 and I2 are
soluble in it. So, chloroform, trichloroethylene, perchloroethylene and maybe even ligroin/petroleum ether could do the job.
Solvents like methanol, ethanol, isopropanol and most likely also acetone will not do the job. I expect that they react with SnI4, giving rise to
hydrous SnO2 and some partially iodinated hydrocarbon.
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itchyfruit
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I wasn't going to use tincture of iodine,just the same solvent, but that won't do it either.
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entropy51
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Woelen predicts CHCl3 is a likely candidate and CHCl3 is one of the easiest solvents for amateurs to make from OTC ingredients. Acetone and Ca(OCl)2
or bleach. And CHCl3 is not flammable. Making the chloroform is a nice experiment in and of itself. Several threads here discuss preparation of
CHCl3.
If you have a solvent containing CH2Cl2 you can distill that out. Magpie has described how he did it in another thread.
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UnintentionalChaos
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| Quote: Originally posted by UnintentionalChaos |
It means the off-topic crud was split off and made into a seperate thread...in this case, moved directly to detritus.
I have some perchloroethylene...and iodine, and tin. I could give this a try.
[Edited on 9-19-09 by UnintentionalChaos] |
I posted over in the actual thread, since this one *should* be about CS2 only. It works, by the way, but is less convenient.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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itchyfruit
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Good point. i would still like some carbon disulphide, as i quite often see it mentioned in practical text books so i'm sure it would be useful to
have just a little.
I do remember seeing a thread about purifying paint stripper.
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panziandi
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Itchy:
Dichloromethane is not flammable, so your hood should be ok, in fact I use this a lot on the bench (as opposed to "in a hood"), chloroform and carbon
tetrachloride are alternatives. If making tin tetra-iodide, dichloromethane, chloroform, carbon tetrachloride, trichloroethane, tri- and
tetrachloroethylene (I suspect!), benzene, toluene (and xylene?) and ether would also be suitable solvents.
The preparation is EASY and you can prepare and purify by recrystalisation and even perform a mp test with 3 hours!
I would HIGHLY suggest the use of DCM (cheap and easy to obtain, be it OTC in paint stripper or from online suppliers) since it is not flammable but
is easily evaporated/removed. Otherwise I would suggest >Xylene>Toluene>Chloroform>Trichloroethane>>Carbon
tetrachloride>Benzene>Diethyl ether>Carbon disulphide...
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itchyfruit
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My paint stripper is 10% methanol,would it still be ok?
I take it you didn't see anything suitable while you were here, i have Xylene heptane and styrene.
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Jor
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I don't think so. SnI4 reacts with it to tin methoxide I think, but I'm not sure!
And I;m also not sure if you seperate them by distillation, as AFAIK MeOH and DCM form an azeotrope, but again this is a vague memory, and I could be
wrong.
Try distilling it.
Oh and by the way, for any of those in Europe, unable to buy from chemicals suppliers, you should really stock up on paint stripper, as they will soon
be banned:
http://www.sciencemadness.org/talk/viewthread.php?tid=3254&a...
Scroll down.
DCM is only of the most useful solvents I know (dissolves a lot, highly volatile, inert), and for me (I have a hood) also one of the safest
(non-flammable).
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panziandi
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Styrene wouldn't be suitable. Xylene should be ok...
Fisher has this to say regarding SnI4:
"Solubility in water:
decomposes
Solubility in other solvents:
soluble in alcohol, benzene, chloroform, ether and carbon disulfide"
Now then if you have xylene, and you also have di-isopropyl ether if I recall correctly, both of them should be suitable. Heptane/petroleum I suspect
would work ok. But the solubility of the product maybe lower. I do not recall you having anything else suitable. Dichloromethane you should be able to
acquire cheaply and fairly easily frm some UK suppliers you already use. And it IS worth getting a 2.5L winchester of this versatile solvent!
Alternatively purify your paint stripper! CaCl2 will selectively absorb water and methanol, firstly distil the DCM off (fractionating column) then
with the distilate, stand over CaCl2 overnight, filter, and the redistill the DCM to obtain the pure DCM which should then be dry and free of
methanol. CaCl2 is CHEAP and chips and can be had form any DIY shop as a dehumidifier refill (if you dont have any of the stuff already)... and whilst
you are there pick up a couple more tins of paint stripper 
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itchyfruit
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I'll try the di isopropyl ether and the xylene and compare the results
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panziandi
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great idea! good luck be sure to report back yields! are you able to check for peroxide in you ether before you do the experiment?
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