Excess of iodine, and no sodium thiosulfate avail.

[jammin]

My friend read geez's excellent posts, one talks about post reaction cleanup. He has done an LWR (10g e.hcl, 14i, 4rp, 10ml dh20) and since:
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"If the fluid is reddish-orange, but the red phosphorous falls like bricks to the bottom, you likely have an excess of iodine present in the reaction fluid"
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is true, he tried to boil the sollution but i didnt help much. Tried to wash with NP, _several_ times, but all NP turned piss yellow.


Tried to boil again for 15 min, didnt help much either. Tried to get sodium thiosulfate without success. Aquarium stores here dont carry any brand that contains this.


What should he do?
He obviously cant wash for ever in NP, the sollutuion just seems to dilute minute amouts of i2...

Everything else has gont according to plan, swim dosent want i2 in is product...

[wareami]

If there aren't any photo supply stores in the area(completely legal...sold as hypo and is most commonly used as a fixing agent for films and prints in the photography industry), don't sweat it. If after gently refluxing the post-rxn solution for 10 min, there is still some free iodine present it will be left behind in the basified solution during work-up.

[jammin]

He has now basified the sollution...
Seemed like som soilds formed(??), but the are in sollution now. Ah, well, he now has about 100ml of the NaOH / rxn fluid, and this was for a 10g rxn. How much tolly shouuld he use for extraction? Seems geez suggests 3x 200 ml?


But his sep funnel is only 125ml...

Can he reduce the amount of rxn fluid?
Or does he need at least these volumes?

[wareami]

The sep funnel is too small for work-up.
Use a beaker or a pyrex measuring cup. An-E-Thing that has a pour spout(glass).
Do three extracts of the reactants(filtering red)
Either do three NP pulls off each extract after basifying  or combine all three extracts in one and proceed to do NP pulls off that until AWE is retrieved!
Ibee does the three separate extracts and 3 NP pulls off each. Each NP pull is 75ml NP.
Add more base splashwise between NP pulls.

[jammin]

>The sep funnel is too small for work-up.
Use a beaker or a pyrex measuring cup. An-E-Thing that has a pour spout(glass).

Ok, he has a beaker he can use...

>Do three extracts of the reactants(filtering red)

This i didnt get?
Filtering red?
He already filtered the red and based it. Totqal volume is about 100ml.

>Either do three NP pulls off each extract after basifying 
or combine all three extracts in one and proceed to do NP
pulls off that until AWE is retrieved!


He'll try 3 75 NP pulls, but how does he mix this in a beaker?
Just stirr with a glas rod, or in a bottle first then shake?

Thanks a lot man, i donno what he would have done without geez and your own posts!

[place]

Wouldn't a key plunk clean up get rid of the I₂?

[wareami]

This i didnt get?
Filtering red?
He already filtered the red and based it. Totqal volume is about 100ml.

If only one 100ml of dh2o was added to the reactants in rxnflask all at once(filtering red), chances are there are still more goodz left behind.
Add more dh2o to the rxn flask to get the last.

He'll try 3 75 NP pulls, but how does he mix this in a beaker?
Just stirr with a glas rod, or in a bottle first then shake?

Okay...SWIJ got basified solution(BS ...100ml:
Add NP and stir and let sit for 10-20min stirring now and then.
Pour off NP.
Add more NP and base again splashwise, stir...pour off NP....
Repeat until AWE is gotten.
For 100ml BS....it will take more than three 75ml NP pulls

Avoid shaking NP and BS as it will trap BS and h2o molecules(tinybubbles) in the NP and it takes a while to settle out.


place: kerplunking works as well but Ibee only does it when needed....(gaaked)