The best alternative to gassing mesc hcl - a tek

[Touche Guevara]

Any thoughts as to a good use for the limo/acetone mix that one would be left with? Unless there's a way to separate the acetone, perhaps by distillation, it seems that this tek would be somewhat wasteful.

You should be able to separate the limo from the acetone by adding water, mixing, letting it separate and decanting a couple times. The acetone should move into the water layer.

:!:
This calls for experimentation!

Thanks, narmz

 

[Infundibulum]

Any thoughts as to a good use for the limo/acetone mix that one would be left with? Unless there's a way to separate the acetone, perhaps by distillation, it seems that this tek would be somewhat wasteful.

You should be able to separate the limo from the acetone by adding water, mixing, letting it separate and decanting a couple times. The acetone should move into the water layer.

:!:
This calls for experimentation!

Thanks, narmz

Nah, not really experimentation. Washing the NP with water is a well-tested practise for cleaning away acetone from limonene, xylele, toluene, DCM, naphtha, ether etc.

 

[dg]

very inertesting thread! awesome

so i modified lorax's tek years ago...

i'll post a full write up when i can take some more pics

 

[antichode]

holy shit!! :shock:



thats impressive

Is it a sulfate?

 

[Crystalito]

As an alternative to gassing with HCl, couldnt one drop dry ice (solid CO2) in the non polar solvent?

Could that serve as a "sort-of" gassing, plus cool down the solvent for less solubility of mesc in it?

 

[narmz]

As an alternative to gassing with HCl, couldnt one drop dry ice (solid CO2) in the non polar solvent?

I'm not entirely sure about this, but I think you need H2O to form the carbonic acid necessary to form the carbonate salt. Simply adding dry ice I wouldn't think could cause carbonic acid to form in a non-polar solvent, I think water must be involved somewhere.

 

[PlainCoil]

SWIM tried dropping dry ice into limonene with decent success. He didn't seal the cap all the way for fear of CO2 buildup and explosion, and he added distilled water to retrieve the salted alkaloids (he couldn't filter as he didn't see any solids form in the limonene, though it did become cloudy as the CO2 bubbled through it).

Perhaps the addition of distilled water formed carbonic acid and this was the reason for his success?

 

[Touche Guevara]

A friend just called me and said he's having trouble with Phlux-'s "best alternative to gassing" tek. Says after adding the anhydrous HASA to the limonene, he's getting separation of layers with some bubbles in between.

I told him he probably didn't dehydrate the HASA enough. Can anyone speculate as to whether that's probably what happened? Assuming the presence of layers equates to the presence of H2O. How long should the HASA be mixed with anhydrous Mg2SO4? Is there a visual cue to tell when it's properly dehydrated?

Gratitude and best wishes!

 

[Infundibulum]

SWIM tried dropping dry ice into limonene with decent success. He didn't seal the cap all the way for fear of CO2 buildup and explosion, and he added distilled water to retrieve the salted alkaloids (he couldn't filter as he didn't see any solids form in the limonene, though it did become cloudy as the CO2 bubbled through it).

Perhaps the addition of distilled water formed carbonic acid and this was the reason for his success?

adding just dry ice in limonene pulls won't salt anything; just as narmz said, CO2 needs to be dissolved in water so as to make carbonic acid, i.e. the acid that will eventually salt alkaloids. Any precipitation seen when dry ice is added to just limonene is not salted alkaloids. It is literally anything that precipitates out of the limonene that is not soluble in it due to the very low temperature; it may be fats, oils, freebase mescaline, even frozen limonene chunks. Clouding alone means not much.

Now, if water was added then carbonic acid could form and salt the good stuff, as SWIY apparently did.

 

[Infundibulum]

A friend just called me and said he's having trouble with Phlux-'s "best alternative to gassing" tek. Says after adding the anhydrous HASA to the limonene, he's getting separation of layers with some bubbles in between.

I told him he probably didn't dehydrate the HASA enough. Can anyone speculate as to whether that's probably what happened? Assuming the presence of layers equates to the presence of H2O. How long should the HASA be mixed with anhydrous Mg2SO4? Is there a visual cue to tell when it's properly dehydrated?

Gratitude and best wishes!

Does your friend has specifics on the amount of materials he used? e.g. how much HCl solution of what percentage in how much acetone and how much magnesium sulfate was added?

It is a matter of a couple of straightforward calculations to find how much MgSO4 to add to ensure the minimum amount of water present. Just remember that anhydrous magnesium sulfate absorbs its own weight in water. What your friend sees is most likely water and limonene and emulsion maybe?

 

[Touche Guevara]

Update: Here is a pic of what the situation looks like.

He's trying a hot water bath, says it seems to be releasing some of the bubbles.

 

[soulfood]

So are many people using this method?

I tried it out today and now I'm just watching the precips slowly forming. Seems to beat waiting for water to evaporate that's for sure.

 

[soulfood]

So....

any idea of how to go about collecting these micro-crystals?

They passed right through my filter.

 

[w0mbat]

very inertesting thread! awesome

so i modified lorax's tek years ago...

i'll post a full write up when i can take some more pics

dg we are still waiting for this writeup!!!!! The crystals look good, but were they active?

 

[antichode]

dg we are still waiting for this writeup!!!!! The crystals look good, but were they active?

there isn't anything else that could possibly be, but a refined careful titration to pure mesc

 

[Touche Guevara]

A friend just called me and said he's having trouble with Phlux-'s "best alternative to gassing" tek. Says after adding the anhydrous HASA to the limonene, he's getting separation of layers with some bubbles in between.

I told him he probably didn't dehydrate the HASA enough. Can anyone speculate as to whether that's probably what happened? Assuming the presence of layers equates to the presence of H2O. How long should the HASA be mixed with anhydrous Mg2SO4? Is there a visual cue to tell when it's properly dehydrated?

Gratitude and best wishes!

Does your friend has specifics on the amount of materials he used? e.g. how much HCl solution of what percentage in how much acetone and how much magnesium sulfate was added?

It is a matter of a couple of straightforward calculations to find how much MgSO4 to add to ensure the minimum amount of water present. Just remember that anhydrous magnesium sulfate absorbs its own weight in water. What your friend sees is most likely water and limonene and emulsion maybe?

Finally had some time to go over this with the guy. He realized that he'd dried the Acetone/HCL but not the limonene! I gave him a kind lecture about making sure to read more carefully when attempting such things.

 

[acacian]

hey Phlux I noticed the link to the original tek you posted isn't working. I was just wondering if you could give any advice on the amount of acetone you used here and how much HCl you added to it before anhydrating? I will be adding my HCL to already anhydrated acetone so I am guessing I'll still need to re-anhydrate it due to the water present in the HCL? My main concern here is whether using too much HCL will have any negative effect on the precipitates?

what is your opinion on solvent ratio to maximise precipitation? is it similar to dmt where the less solvent you have the easier it will precipitate?

thanks

 

[dg]

link works fine if you are a nook member...

here is another method inspired by Lorax- but simpler in application

simple titration, and dual solvent crystalization - Preparation - Welcome to the DMT-Nexus