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Sulaiman
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CS2 is rather pricey;
http://onyxmet.com/?route=product/product&filter_name=ca...
If someone could point me to a competitive source that ships to UK amateurs I'd be grateful.
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DavidJR
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You could maybe try Rathburn Chemicals as they list CS2 on their site: http://rathburn.co.uk/product-list/
You'll have to email them to get a quote and order. They specialise in very high purity solvents so it might not be cheap but it's worth asking. I've
ordered HPLC-grade solvents from them before and they are friendly and helpful and willing to sell to individuals/sole traders.
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Sulaiman
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Thank You !
I just telephoned Rathburn Chemicals,
RG2027 glass-distilled Carbon Disulphide, 500ml £20 ++
I am in the process of registration now.
Not only a competitive source but a new source that ships to amateurs,
with 30-day credit.
Shipping is £14 for up to one pallet of chems...
Thanks so much.
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Herr Haber
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I've got enough CS2 to pick up where your bottle left you.
Trouble is, I have to distill enough HNO3 by the end of the weekend to dissolve 1.5kg of silverware...
I might give it a try as I also have red P and a few miligrams of impure white P.
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Sulaiman
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Excellent,
because I'm not going to buy any chemicals for a while due to lack of spare cash 
UPDATE:
Rathburn chemicals have replied ... I can order as soon as funds permit 
[Edited on 1-11-2018 by Sulaiman]
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artemov
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I have chemicals envy of all of you ...
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Sulaiman
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minor PI3 update
I just examined the 250ml bottle with c60ml mixture as described earlier above;
. the blue plastic GL45 cap is very discoloured and bulging a little
. there is very little sediment 
the volume of sediment is visibly less than the starting volume of the redP alone ...
either all of the iodine and some of the redP has dissolved in the CS2
or there has been a significant quantity of redP consumed,
and as I have been reminded a few times above ... 'redP is not soluble in CS2'
... something good must be happening.
After getting 'dressed-up' for the unexpected,
with the camera rolling I carefully opened the bottle cap and
... absolutely nothing dramatic happened.
Very little internal pressure (Ta<<20oC) but some 'smoke'.
I re-capped the bottle and I'll check it sometime later - nearer to Xmas.
So it appears that although redP is 'insoluble' in CS2,
the minute solubility that it does have enables the reaction to proceed, very slowly, hopefully to completion.
Other than glimpses of sediment I really can not determine what is happening by any noticeable visible change.
Considering that the reactants and product and solvent each have their own safety hazards,
so far, this has been one of the gentlest reactions that I've ever done.
My main concern now is;
what the heck am I going to do with the PI3 ?
and how do I recover my CS2 ?
... t.b.d.
CAUTION : Hobby Chemist, not Professional or even Amateur
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artemov
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Quote: Originally posted by Sulaiman  | I just examined the 250ml bottle with c60ml mixture as described earlier above;
. the blue plastic GL45 cap is very discoloured and bulging a little
. there is very little sediment
the volume of sediment is visibly less than the starting volume of the redP alone ...
either all of the iodine and some of the redP has dissolved in the CS2
or there has been a significant quantity of redP consumed,
and as I have been reminded a few times above ... 'redP is not soluble in CS2'
... something good must be happening.
After getting 'dressed-up' for the unexpected,
with the camera rolling I carefully opened the bottle cap and
... absolutely nothing dramatic happened.
Very little internal pressure (Ta<<20oC) but some 'smoke'.
I re-capped the bottle and I'll check it sometime later - nearer to Xmas.
So it appears that although redP is 'insoluble' in CS2,
the minute solubility that it does have enables the reaction to proceed, very slowly, hopefully to completion.
Other than glimpses of sediment I really can not determine what is happening by any noticeable visible change.
Considering that the reactants and product and solvent each have their own safety hazards,
so far, this has been one of the gentlest reactions that I've ever done.
My main concern now is;
what the heck am I going to do with the PI3 ?
and how do I recover my CS2 ?
... t.b.d. |
Fantastic!!! I dun have CS2, so I'll probably try it with toluene (or hexane).
What's the color of the solution? Any pics?
Are you able to dry a few drops of the clear solution and obtain dry red PI3?
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Sulaiman
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A quick video of the appearance, nothing interesting. https://www.youtube.com/watch?v=WngVdTs9DME
CAUTION : Hobby Chemist, not Professional or even Amateur
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artemov
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Wow thanks! Nice dark red, and nice weather!
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Sulaiman
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| Quote: Originally posted by Herr Haber | I've got enough CS2 to pick up where your bottle left you.
Trouble is, I have to distill enough HNO3 by the end of the weekend to dissolve 1.5kg of silverware...
I might give it a try as I also have red P and a few milligrams of impure white P. |
Unless you need PI3 please do not waste your time and reagents,
it is just a simple combination synthesis.
(SM Wiki: http://www.sciencemadness.org/smwiki/index.php/Phosphorus_tr... )
I guess that refluxing would have the job done in minutes.
Just about all of the redP has now 'gone'.
Pouring the liquid from the 250ml bottle into a 100ml bottle I could smell/taste :
. the CS2 (impurities),
. hints of both iodine and phosphorus,
. an unfamiliar strong nasty smell.
Even in cold dry air there was 'smoke'
Today I completed the construction of my upgraded water cooler/chiller module
(now 4x TEC@c6V, was 2x TEC@c12V)
so soon I hope to recover the CS2 and PI3.
[Edited on 21-11-2018 by Sulaiman]
CAUTION : Hobby Chemist, not Professional or even Amateur
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Herr Haber
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Thanks Sulaiman,
No need for it but I'm following the thread because it's interesting.
3 weeks later finally the last of my silver is dissolved. Spent the last week watching a 300 grams ingot go into solution...
Thanks for sharing your results and congratulations of your water cooler 
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Sulaiman
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... update ...
I have not yet tried to recover the CS2 from my (assumed) PI3,
the mixture was stored with a cork covered in many layers of cling film plastic.
(I did not expect such a long storage period)
Here is the result, on the right;
On the left are a few iodine prills in distilled water as a colour reference for saturated iodine solution,
the stopper seems to have absorbed more iodine than the water
(The stopper was white and never in contact with the liquid,
only iodine vapour that passed through, then evaporated from, the water, could be responsible).
i.e. water does not reduce the evaporation rate to zero.
P.S. My water cooler is now two similar modules,
each module has two fan/heatsink/TEC and one 40x40 mm water tank.
At high water flow rate it makes little difference if the two modules are plumbed in series or parallel.
Progress suspended until probably next year due to relocation with expected ambient temperature 'upgraded' to 22 to 32 oC
[Edited on 20-4-2019 by Sulaiman]
CAUTION : Hobby Chemist, not Professional or even Amateur
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