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dobeid
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Bubbling dry HCl gas through a extract
Can someone explain exactly what the process is for "bubbling dry HCl gas through an extract". I can not seem to find step-by-step instructions. If
this process is posted somewhere, pointing me to the web site or explanation would be greatly appreciated.
Thanks
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kclo4
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Well, what is it you are doing exactly, or are wanting to achieve?
Are you referring to precipitating an alkaloid salt from a polar solvent?
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solo
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I guess he wants to make a salt.....an HCl salt, so have some HCl in separatory funnel and drip it into some H2SO4....then have an exit from where
all this is happening attached to a hose that runs through a drying tube and then into the solution you wish to chlorinate.......solo
It's better to die on your feet, than live on your knees....Emiliano Zapata.
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Hulagu khan
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Swim would like to know from the friendly Bees if he would need to boil/evaporate some of the solvent (ether) in the solution before doing the
bubbling process mentioned above or will the HCL gas evaporate the solvent and turn the solution into crystals (pardon me if the question seems dumb,
swim is still very wet behind the ears when it comes to different types of synthesis’ and he has been learning a lot from the posts on this forum
from various Bees
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Abromination
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Sounds like cookery, but I could be wrong. Its cheapest to dropwise add hydrochloric acid to anhydrous calcium chloride, leading the gas thorough a
washer full of 98% sulfuric acid or another suitable drying agent (maybe a bit unnecessary, the calcium chloride should remove most water) and from
there bubbling into your “extract.”
It would of course help to know what that “extract” is though.
List of materials made by ScienceMadness.org users:
https://docs.google.com/spreadsheets/d/1nmJ8uq-h4IkXPxD5svnT...
--------------------------------
Elements Collected: H, Li, B, C, N, O, Mg, Al, Si, P, S, Fe, Ni, Cu, Zn, Ag, I, Au, Pb, Bi, Am
Last Acquired: B
Next: Na
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G-Coupled
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Quote: Originally posted by Hulagu khan  | | Swim would like to know from the friendly Bees if he would need to boil/evaporate some of the solvent (ether) in the solution before doing the
bubbling process mentioned above or will the HCL gas evaporate the solvent and turn the solution into crystals (pardon me if the question seems dumb,
swim is still very wet behind the ears when it comes to different types of synthesis’ and he has been learning a lot from the posts on this forum
from various Bees |
You want to generate 'dry' (as in no water) HCl gas, as detailed in multiple posts here already, and when this is bubbled through the solvent (Diethyl
Ether?) containing the freebase of your desired product , the Hydrochloride salt of your product will form which is insoluble in the Ether so it will
'salt out' of solution in the form of many tiny crystals. You then evaporate/filter/recrystallise, or whatever.
You want to keep water out of the process as the salt form of your reaction product is almost certainly soluble in water, so you will lose product,
the more water is present.
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Hulagu khan
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Abromination and G-Coupled, Swim is so grateful for your Superbee input and swim would like to clarify that he joined the forum a few hours ago and
though a lot of posts on the forum have been helpful to swim but he just needed to know the missing piece of the puzzle that you just assisted with.
Swim can’t find words to show his gratitude.
[Edited on 27-12-2019 by Hulagu khan]
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Texium
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@Hulagu khan: I see that you are new here. Please read the forum guidelines: https://www.sciencemadness.org/whisper/viewthread.php?tid=19...
How you spend your personal time and what you use information here for is none of my business, but we don’t tolerate “swim” talk here. In the
future please refrain from it, or you can expect to find your posts in Detritus.
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Abromination
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I am not sure as to what “swim talk” is, anyone care to inform me? Either way I regret replying to this blatant spoon feeding in the first place.
List of materials made by ScienceMadness.org users:
https://docs.google.com/spreadsheets/d/1nmJ8uq-h4IkXPxD5svnT...
--------------------------------
Elements Collected: H, Li, B, C, N, O, Mg, Al, Si, P, S, Fe, Ni, Cu, Zn, Ag, I, Au, Pb, Bi, Am
Last Acquired: B
Next: Na
-------------- |
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Hulagu khan
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My apologies @Texium, I assumed it was common for someone who is new to such a forum to refer to themselves as a swim. I appreciate the heads up, I
saw it being used by some members who referred to themselves as being new members. I will go through the guidelines to ensure a similar thing never
happens again.
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G-Coupled
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SWIM = 'Someone Who Isn't Me' - not so much to do with account newness, more it was used on forums as a kind of 'can't (legally) prove it was me' kind
of thing.
Seemed to die out like a decade ago or so, but one might still come across it in old archived forum threads etc.
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Yttrium2
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I've tried several methods out in the woods...
Hcl + sulfuric made a big cloud of hcl
Salt + sulfuric was more controllable
Al + HCL aq took off like a rocket..
Hcl + calcium chloride - I forget.
Hcl + calcium chloride from the dollar store is your best option .
Now for contraptions, I used to use a water bottle with a polypropylene hose in the center. I would add sulfuric acid and table salt. The bottle would
be squeezed as I inserted the tube to the liquid to be gassed'
And retracted so fresh air could be sucked in
Squeezed again when inserting the tube.
In the future I'll use calcium chloride and hcl aq, though I don't remember how quickly this takes off. It's the cheapest route.
I wonder how much the moisture affects the yield, in addition...
Wear Goggles
[Edited on 12/28/2019 by Yttrium2]
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morganbw
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| Quote: Originally posted by Yttrium2 | I've tried several methods out in the woods...
Hcl + sulfuric made a big cloud of hcl
Salt + sulfuric was more controllable
Al + HCL aq took off like a rocket..
Hcl + calcium chloride - I forget.
Hcl + calcium chloride from the dollar store is your best option .
Now for contraptions, I used to use a water bottle with a polypropylene hose in the center. I would add sulfuric acid and table salt. The bottle would
be squeezed as I inserted the tube to the liquid to be gassed'
And retracted so fresh air could be sucked in
Squeezed again when inserting the tube.
In the future I'll use calcium chloride and hcl aq, though I don't remember how quickly this takes off. It's the cheapest route.
I wonder how much the moisture affects the yield, in addition...
Wear Goggles
[Edited on 12/28/2019 by Yttrium2] |
Yields? Of what.
Be careful of those woods.
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Hulagu khan
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| Quote: Originally posted by G-Coupled | SWIM = 'Someone Who Isn't Me' - not so much to do with account newness, more it was used on forums as a kind of 'can't (legally) prove it was me' kind
of thing.
Seemed to die out like a decade ago or so, but one might still come across it in old archived forum threads etc. |
I highly appreciate the heads up G-Coupled and I have noticed some of the posts on the forum are +/-15yrs old. I appreciate your input.
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draculic acid69
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| Quote: Originally posted by Yttrium2 | I've tried several methods out in the woods...
Hcl + sulfuric made a big cloud of hcl
Salt + sulfuric was more controllable
Al + HCL aq took off like a rocket..
Hcl + calcium chloride - I forget.
Hcl + calcium chloride from the dollar store is your best option .
Now for contraptions, I used to use a water bottle with a polypropylene hose in the center. I would add sulfuric acid and table salt. The bottle would
be squeezed as I inserted the tube to the liquid to be gassed'
And retracted so fresh air could be sucked in
Squeezed again when inserting the tube.
In the future I'll use calcium chloride and hcl aq, though I don't remember how quickly this takes off. It's the cheapest route.
I wonder how much the moisture affects the yield, in addition...
Wear Goggles
[Edited on 12/28/2019 by Yttrium2] |
U forgot to try calcium chloride and h2so4 which provides twice as much dry HCl compAred to HCl +Al which equals wet gas.
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BromicAcid
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I ignored it the first time but since it was brought up again:
6HCl (aq) + 2Al ---> 2AlCl3 (hydrated) + 3H2
No hydrogen chloride
Edit: The exotherm of the reaction may volatilize some already there but you're not forming it.
[Edited on 1/15/2020 by BromicAcid]
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draculic acid69
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HCl +Al = definitely large amounts of HCl gas whether or not it's just evolved bcoz of a thermal increase caused by the HCl+Al=alcl3+H2 or not it
definitely releases HCl gas
Wet gas but gas none the less.lots of Al is left over after it usually.so the alcl3 formation is rather minor I'd say.i don't think any usable amount
of hydrogen could be separated from the HCl gas no matter how much bubbling and scrubbing u put it through. It's predominantly HCl gas.
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draculic acid69
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And yes I understand that it's not really forming HCL but that's not really a relevant point in this post.
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BromicAcid
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Relevant in this post? This is a chemistry forum. Ignorance like that should not be allowed to pass unchecked. In this case you might as well just
heat the hydrochloric acid on a hot plate.
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OldNubbins
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More like a soggy cloud of mist containing some HCL due to all the hydrogen bubbles. But I could be wrong because sounding confidently wrong
is just..... silly....
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Tsjerk
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What works nicely without having to deal with any gas is adding concentrated HCl to ether with CaCl2 on the bottom. The HCl will sink to the bottom
where the water is absorbed by the CaCl2. If done slowly all HCl will dissolve in the ether, qiving a solution of dry HCl in ether. It is a good as
quantitive so you can calculate the amount of HCl needed, and the ether can be decanted or filtered.
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draculic acid69
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Have either of you ever actually tried it.i have.it worked.so I don't really see how it could in any way be wrong.
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draculic acid69
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| Quote: Originally posted by BromicAcid | | Relevant in this post? This is a chemistry forum. Ignorance like that should not be allowed to pass unchecked. In this case you might as well just
heat the hydrochloric acid on a hot plate. |
U could just put it on the hotplate but it would be extremely ineffective compared to the Al foil method.and there'd be way too much water and way too
slow.
Whether it's formed or evolved is not really something to give a shit about when gassing something
[Edited on 15-1-2020 by draculic acid69]
[Edited on 15-1-2020 by draculic acid69]
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Abromination
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| Quote: Originally posted by draculic acid69 | | Quote: Originally posted by BromicAcid | | Relevant in this post? This is a chemistry forum. Ignorance like that should not be allowed to pass unchecked. In this case you might as well just
heat the hydrochloric acid on a hot plate. |
U could just put it on the hotplate but it would be extremely ineffective compared to the Al foil method.and there'd be way too much water and way too
slow.
Whether it's formed or evolved is not really something to give a shit about when gassing something
[Edited on 15-1-2020 by draculic acid69]
[Edited on 15-1-2020 by draculic acid69] |
You dont evolve any extra gas through aluminium then by heating. The only reason HCl would be evolved through the reaction of HCl and aluminium would
be through heating from the exothermic reaction.
If you want to explain your reasoning, we would here it.
[Edited on 1-15-20 by Abromination]
List of materials made by ScienceMadness.org users:
https://docs.google.com/spreadsheets/d/1nmJ8uq-h4IkXPxD5svnT...
--------------------------------
Elements Collected: H, Li, B, C, N, O, Mg, Al, Si, P, S, Fe, Ni, Cu, Zn, Ag, I, Au, Pb, Bi, Am
Last Acquired: B
Next: Na
-------------- |
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morganbw
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The Al in HCl may not produce HCl gas, I get it, the chemistry thing
I do know that some shake and bake producers use this method for their gas.
Carried over in spite of the bad chemistry, I guess.
Good method, absolutely not, but they do get crystals.
Shake and bake, good method, horrendous from a chemist point of view, but they do get crystals.
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