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HCl+MeOH instead of gasing?

Started by methlab, January 18, 2004, 04:06:00 AM

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methlab

Hi! This time i got white (tooth-?)paste in my beaker after gasing. I am unable to perfom this step. A post says, that one can also drip in a HCl/Methanol mix instead of gasing. Who has done this allready? Have an recipe ready for me?

methlab

I did an Acid/Base extraction to clean out unwanted stuff, then i did used a different gasing technique. This time i did it with Sulfuric Acid as 'Rhodium' and 'Stuff' told me. I will never do this with CaCl2, it seems that i am too silly to do it like that. Now everything is perfect and i am going to eat this stuff now... :)

Mercury

How did you set up the gasser with CaCl2? What did you do exactly?

methlab

1l 3-neck flask, left stoppered, right 250ml additionfunnel with sulfuric acid, condenser on top filled with CaCl2,  stoppered vacuumadapter attached, PE hose with glasspipette on vacuuminlet. Could not get pure NaCl, had to buy NaCl (Tablesault, but with 0,004% Calcium inside). NaCl was put into 3-neck flask and a few milliliter of muriatic acid dropped in. Addition funnel controlled the gasproduction.
I am using labgrade MgSO4 (<4 mol H20) dried for 2h at 200C in mother's baking-oven. So this could not be the problem. Must the hose also be anhydrous ? Now i build a ghetto-lowbudget-gasing-mashine. A plastic bottle with one hoe on top. Hose leads to glas with conc. sulfuric acid, 2cm space to top. Second hose on top with glasspipette. I throw in a few ml of sulf. acid into NaCl bottle and immediatle attach tophose. When i compress first bottle, gas is pressed into sulf. acid bottle, bubble come out of sulf, acid and go through hose into my lovely freebase. That's how it worked...
Greetings from europe :)

hest

UTFSE

Methanolic HCl is the way to doo it. Just boubble HCl throug cold methanol. You will end with something like an 5M solution.