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Gasing in the Al/HG.
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DjTime
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Joined: 18 Feb 2005
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Sat May 14, 2005 7:21 am
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SWIM has had poor yeilds latley. He is certain that the Al/Hg is going as it is supposed to. All evolution of the reactions seems to go as planned. However when SWIM gasses the solution at the end. In his dream at most of the last 4 runs he has gotten about 15-30% yeilds. SWIM has ran many of these Al/Hg's before with yeild nearly %75-80. He knows what looks right. But swim ponders the question. Can the way your setup is rigged or the type of ingredients used to make the gas effect your end result? SWIM uses a 2L 2Neck RBF he pours NaCL on the bottom, wets with muratic. Places an addition funnel with virgin sulfuric acid in it bought from a local grocery and store chain. Then he drips in the sulf, on top of the HCL and has it going up through an adapter to a take off adapter then down through a west condenser into his jar of crap. Any ideas?
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anime

Joined: 13 Apr 2005
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Sun May 15, 2005 3:07 am
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Drop the HCl into the Sulfuric acid, your gas is probably still wet. Also use CaCl2 or MgSO4 to dry the gas as it passes through. IMO its best to gas a liter of anhydrous IPA that way you don't have to be exposed to HCL gas everytime you perform a reduction.
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Bumblebee

Joined: 26 Mar 2005
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Sun May 15, 2005 4:28 am
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... and the hcl takes up HCl and you can drip this in to your extract?
fine. how do i know how much HCl is in the IPA solution?
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icecool
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Joined: 16 Feb 2005
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Sun May 15, 2005 4:32 pm
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Wouldn't it be possible insted of letting Al and HgCl2 react with eachother to form hydrogen gas.
To just bubble H2 gas threw an acidic solution of P2NP in alcohol.
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brain
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Joined: 08 Mar 2005
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Sun May 15, 2005 6:12 pm
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icecool wrote:
Wouldn't it be possible insted of letting Al and HgCl2 react with eachother to form hydrogen gas.
To just bubble H2 gas threw an acidic solution of P2NP in alcohol.


widouth Ni catalis - no Smile i tryed it eawen in high presure Smile with good Ni [w-12 nickel or w-6] - its in good yelds ! in lower presures ...

when Al react with acid/h2o - there is formed H (atom) - form of hydrogen, whih is good reductin reagent, bubling H2 (molecue) gas -this form of hydrogen is inactive in these case-when widouth Ni for example Smile
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DjTime
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Joined: 18 Feb 2005
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Mon May 16, 2005 9:48 am
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So SWIM followed advice. SWIM ran gassing like this. 2L, 2 Neck RBF (24/40) setup. With 500mL addition unnel fitted to one neck with 250mL of HCL in it. The other neck was fitted with an distillation adapter, to a vaccum adapter (plugged up take of valve) which had a hose aatached. In the 2L RBF was NaCL wetted with sulfuric acid. Had an MgSO4 napkin in the line to dry gas. Dripped in HCL over the sulfuric. SWIM had excellent results. SWIM netted 17.4G. Thanks. Peace Out.....
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