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Topic: keeping a solution totally dried (with out oxigen)  (Read 1392 times)

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Offline CrazyGoat

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keeping a solution totally dried (with out oxigen)
« on: December 28, 2020, 04:59:42 AM »
 
I wanna make a solution of anhydrous zncl2 + anhydrous chloroform, I will mix those two in a glove box under an inert atmosphere:
 I will add them to a 1l flask with some molecular sieves and close them with a rubber septum, so then I can extract the solvent anytime I want with a cannula/syringe for making my dried reactions.

 The question here: Will this be enough for keeping a dried solution of zncl2 on chloroform or eventually will be gaining moisture or O2. (I dont know how effective for this purpose a rubber septum is)

thank you. 

Offline OrganicDan96

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Re: keeping a solution totally dried (with out oxigen)
« Reply #1 on: December 28, 2020, 06:56:37 AM »
i wouldn't keep such a solution for too long, it would probably better to store it in a staus flask or a young's tube as rubber septums can allow moisture in slowly.

Offline rolnor

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Re: keeping a solution totally dried (with out oxigen)
« Reply #2 on: December 28, 2020, 10:55:01 AM »
Molecular sieves can react with ZnCl2. Have you pure CHCl3? Usually it containes some EtOH. I recommend a Schlenk flask, Wernerglas in Sweden has a good model.

Offline CrazyGoat

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Re: keeping a solution totally dried (with out oxigen)
« Reply #3 on: December 28, 2020, 11:06:25 AM »
 staus flask or a young's tube??

may you send me a link to those? I will buy them.

also, the good thing about the rubber was that I could extract it from the flask with a syringe previously refilled with co2 (so no need to open it and exposing it to air)

thanks.

Offline CrazyGoat

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Re: keeping a solution totally dried (with out oxigen)
« Reply #4 on: December 28, 2020, 11:23:16 AM »
Molecular sieves can react with ZnCl2. Have you pure CHCl3? Usually it containes some EtOH. I recommend a Schlenk flask, Wernerglas in Sweden has a good model.

this is the best I have found

Assay (GC, on anhydrous basis)   99.9-100 %
Appearance   Clear colorless liquid
Acidity (as HCl)   0-0.001 %
Residue after evaporation   0-0.0005 % w/w
Stabilizer (Amylene)   0.003-0.006 % w/w
Water (KF)   0-0.005 % w/w

Offline OrganicDan96

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Re: keeping a solution totally dried (with out oxigen)
« Reply #5 on: December 28, 2020, 01:08:53 PM »
this is a straus flask, you connect it to a schlenk line and once the system is under inert atmosphere you remove the tap and place a rubber septum on the outlet and extract solution with a syringe once complete you replace the tap.
https://chemglass.com/flasks-storage-straus-airfree-schlenk?AspxAutoDetectCookieSupport=1

Offline rolnor

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Re: keeping a solution totally dried (with out oxigen)
« Reply #6 on: December 28, 2020, 02:11:16 PM »
It is also called Schlenk in the ad. The bottle I suggest has a flat bottom and is superior I think.
https://www.swab.se/sv/Produkter/Laboratorieglas/General_Glassware/Bottles/Bottle,_Filling_neck_w_screw_cap,_25ml,_thread_GL14?id=00090-50

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