Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
Author: Subject: phosphate polymer
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 2-2-2013 at 17:43
phosphate polymer


A byproduct of the production of HI(aq) using the method of Argox (Rhodium archive) is a phosphate polymer. Using his method I have produced this polymer as shown in the picture below. Argox says that it is insoluble in water and non-polar solvents. I don't have any reason to not believe this but I'm hoping that someone here can suggest a successful solvent. I really would like to recover my 100mL flask. Thanks in advance.

polyphosphate residue.JPG - 84kB




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Vargouille
Hazard to Others
***




Posts: 380
Registered: 16-4-2012
Member Is Offline

Mood: No Mood

[*] posted on 2-2-2013 at 18:15


Well, he says that mechanical action is required, but you might be able to solvate some of it by using hot 38-50% sulfuric acid.
View user's profile View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Offline

Mood: Semi-victorious.

[*] posted on 4-2-2013 at 12:03


Strong base should hydrolyze/depolymerize the phosphates.
View user's profile View All Posts By User
kristofvagyok
National Hazard
****




Posts: 659
Registered: 6-4-2012
Location: Europe
Member Is Offline

Mood: No Mood

[*] posted on 4-2-2013 at 12:31


Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:



I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:

"You can’t become a chemist and expect to live forever."
View user's profile Visit user's homepage View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 7-2-2013 at 13:53


Quote: Originally posted by kristofvagyok  
Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:


This is working and has turned the top 6mm into a liquid gel! For the first 2 days it appeared to do nothing but now today there is clearly degradation of the polymer. I used a 20% KOH in IPA solution.

Thanks to everyone who gave suggestions. I was going to try them all. I just picked kristo's first.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
elementcollector1
International Hazard
*****




Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline

Mood: Molten

[*] posted on 7-2-2013 at 17:18


Try heating to speed things up?



Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
View user's profile View All Posts By User
BromicAcid
International Hazard
*****




Posts: 3227
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline

Mood: Rock n' Roll

[*] posted on 7-2-2013 at 19:24


KOH / IPA for two days, of course it's coming off. You just removed the layer of glass around it :D

In terms of mechanical action give this a go, fill flask 1/2 full of methanol, add some rock salt, swirl and shake the crap out of it. This can work surprisingly well and is easy enough to try. So long as the salt is largely insoluble you can pick your solvent of choice.




Shamelessly plugging my attempts at writing fiction: http://www.robvincent.org
View user's profile Visit user's homepage View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 7-2-2013 at 20:18


Quote: Originally posted by elementcollector1  
Try heating to speed things up?


Heating might well speed things up, especially as it is sitting in my cold garage. But it is making good progress and I'm not in a hurry.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 8-2-2013 at 18:35


Victory was prematurely declared. :( It seems the gel was just precipitated KOH. Back to the drawing board.



The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Organikum
resurrected
*****




Posts: 2329
Registered: 12-10-2002
Location: Europe
Member Is Offline

Mood: busy and in love

[*] posted on 9-2-2013 at 05:59


For speeding up hydrolysis of the polyphosphates - and thats the stuff what else might it be?- you need acidic conditions so the base treatment will have actually hardened the polymer (and eaten some glass). Give it heat an acid and lots of time. And there is no risk you loose your flask to the cure.... ;)


/ORG
View user's profile View All Posts By User
unionised
International Hazard
*****




Posts: 5102
Registered: 1-11-2003
Location: UK
Member Is Offline

Mood: No Mood

[*] posted on 10-2-2013 at 03:55


Quote: Originally posted by Magpie  
Quote: Originally posted by kristofvagyok  
Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:


This is working and has turned the top 6mm into a liquid gel! For the first 2 days it appeared to do nothing but now today there is clearly degradation of the polymer. I used a 20% KOH in IPA solution.

Thanks to everyone who gave suggestions. I was going to try them all. I just picked kristo's first.


Why use IPA rather than water?
View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 15-2-2013 at 11:25


Quote: Originally posted by Vargouille  
Well, he says that mechanical action is required, but you might be able to solvate some of it by using hot 38-50% sulfuric acid.


Quote: Originally posted by Organikum  
For speeding up hydrolysis of the polyphosphates - and thats the stuff what else might it be?- you need acidic conditions so the base treatment will have actually hardened the polymer (and eaten some glass). Give it heat an acid and lots of time. And there is no risk you loose your flask to the cure.... ;)



Yes! Here's the results after a few hours heating with con sulfuric acid:

cleaned RBF.JPG - 120kB

I even recovered an iodine colored working stir bar, which BTW was completely worthless in this application.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User

  Go To Top