Couple pH questions

[cyantific]

With HCL, what is the ideal pH of the acid water (salting solution) ?

If the pH is too low, will this yield dark brown mesc ?

 

[Kash]

Just salt your nonpolar by adding a quantity of water, add alittle hcl and mix for 5 minutes. Check the pH of the salting and if it is less than 5 you have used enough acid. If it is above 5 then add more acid and mix. By titrating like this you dont end up with excess acid in your saltings, and really, you only need to do 1 salting of your total nonpolar.

 

[dg]

With HCL, what is the ideal pH of the acid water (salting solution) ?

If the pH is too low, will this yield dark brown mesc ?

6-7. at ph 7 theoretically its like 99% salted. i shoot for 6.

yes- over acidifying the np leads to brown mesc. as does evapping the water. precipitating the crystals from solution is a nice way to go

 

[cyantific]

6-7. at ph 7 theoretically its like 99% salted. i shoot for 6.

Do you mean ph 6 of the salting solution before mixing with np or after ?

Any tips on how to precipitate vs evaporate?

 

[AlbertKLloyd]

With HCL, what is the ideal pH of the acid water (salting solution) ?

If the pH is too low, will this yield dark brown mesc ?

And in my experience this can lead to yield loss.
I have even seen an odd black material form and crash out in solutions with excess acid that were heated for an extended period.

 

[Kash]

Do you mean ph 6 of the salting solution before mixing with np or after ?

Any tips on how to precipitate vs evaporate?

PH of 5-6 after mixing. SWIM likes to evaporate becuase then you know you get all the goodies out of solution. Then wash in cold MEK to remove impurities, and dissolve in warm acetone/h2o, then chill it to precip splendid crystals.

 

[cyantific]

dissolve in warm acetone/h2o, then chill it to precip splendid crystals.

Can you link to a thread outlining this process? Isn't the mesc souluble in water?

Thanks for the help!

 

[benzyme]

acetone lowers the freezing point of water, thus lowering the solubility.

 

[dg]

dissolve in warm acetone/h2o, then chill it to precip splendid crystals.

Can you link to a thread outlining this process? Isn't the mesc souluble in water?

Thanks for the help!

mescaline sulphate is only mildly soluble in cold water

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

 

[cyantific]

Thank for the link dg, and all your helpful posts. I'm still working with hcl, so I haven't ventured into sulphate yet. After two acetone washes, I'm still looking at some brown hcl. Considering an IPA wash.

To precipitate hcl, could one just mix a bit of water till dissolved then add acetone and freeze?

 

[futura]

Thank for the link dg, and all your helpful posts. I'm still working with hcl, so I haven't ventured into sulphate yet. After two acetone washes, I'm still looking at some brown hcl. Considering an IPA wash.

To precipitate hcl, could one just mix a bit of water till dissolved then add acetone and freeze?

Mesc HCL does not Re-X well with acetone/water as the dual solvent

Acetone/Water Re-X works best for Mesc Sulphate

For Mesc HCL Re-X use an MEK/Water mix.

An IPA wash will clean it up further...but IMHO IPA wash takes something from it that has like an MDMA quality that I really miss in Mesc from extractions...So I have stopped doing that and go for the dual solvent Re-X after careful titration...I start with PH 7 distilled water, Add NP Stir and then check water ph with digital PH pen(it will go UP as mesc alkaloids migrate from NP to water) and add very dilute acid(2%)drop by drop till its back down to PH 7...stir well(I use a Braun Handheld mixer), let sit agin and check and so on...once ph stops dropping all the goodies are out...I actualy do one giant salting cause I use this method(titration)...Try not to get acid into NP if your using d-limo(Ron69tek) or any type of oil(HippieSaladOiltek)

PH 7 gives you 99% of the Mesc, So try not to go lower trying to get that last 1% and youll have a lot less cleaning to do to get your mesc pure.

Next step would be to do the Re-X...Just follow DG's link...his post explains the Re-X very well...Heres a couple Quotes from it "Now in order to recrystallise mescaline sulphate, typically you'd add 5 mL warm water per gram of mescaline, and heat it and add a few drops of water at a time until all the mescaline has dissolved. Then you allow it to cool, and add acetone and pop in the freezer".

"Mesc HCL requires a different mix of solvents and a slightly different method".

 

[cyantific]

Great info Futura, thank you.

For Mesc HCL Re-X use an MEK/Water mix.

Does this sound right... Mix mesc hcl with a bit of water till dissolved then add dry MEK and place in freezer. MEK lowers the solubility of H20 so the mesc will precipitate out.

 

[Kash]

Great info Futura, thank you.

For Mesc HCL Re-X use an MEK/Water mix.

Does this sound right... Mix mesc hcl with a bit of water till dissolved then add dry MEK and place in freezer. MEK lowers the solubility of H20 so the mesc will precipitate out.

In my experience this does not work as water precipitates out of MEK when cooled and then freezes solid. Becuase water and MEK are only partially miscible, cooling only decreases the miscibility.

Along with washing in cold MEK to remove impurities, here is a good method for further cleaning mesc HCL by phlux: Phlux's Quick Mescaline Hcl Recrystallization tek. - Preparation - Welcome to the DMT-Nexus
Basically, mesc hcl is dissolved in a minimal amount of water, then excess acetone added and mixed. Unwanted solids precip out and the solution is evaporated to get the clean mesc hcl. Also mentioned in this thread it says mesc hcl may be dissolved in boiling MEK and then cooled to precip, though it seems unconfirmed.

 

[dg]

Also mentioned in this thread it says mesc hcl may be dissolved in boiling MEK and then cooled to precip, though it seems unconfirmed.

yes thats been confirmed for some years now- i could point you to the original posting via pm if interested

 

[dg]

Does this sound right... Mix mesc hcl with a bit of water till dissolved then add dry MEK and place in freezer. MEK lowers the solubility of H20 so the mesc will precipitate out.

its a bit trickier...

add dry impure mesc hcl to hot mek. if it doesn't all dissolve you may need to add 1-3 drops of water per gram of dried material(minimal water is key here)

now safely(fan/outside) reduce the water/mek until some precip is noted.remove from heat and allow to cool/freeze
filter and wash precipitate

 

[cyantific]

Kash and dg, thank you for the replies. I'm not setup to boil mek, so I'm gonna stick with simple washing. So far I've done a few acetone washes. I'm considering a wash with IPA or MEK but futura has me concerned..... >

An IPA wash will clean it up further...but IMHO IPA wash takes something from it that has like an MDMA quality that I really miss in Mesc from extractions...So I have stopped doing that

Is this a known result of washing with IPA ?

 

[Kash]

add dry impure mesc hcl to hot mek. if it doesn't all dissolve you may need to add 1-3 drops of water per gram of dried material(minimal water is key here)

Interesting... SWIM had water crash out of solution doing this and freezing, though he added a few ml instead of just a few drops that is likely why. Good info!:thumb_up:

 

[cyantific]

On my last pull, the crystals were light green. Does this mean some base/sludge transferred into the NP? How can I clean this up?

 

[Kash]

What solvent did you use? That looks very odd.

 

[cyantific]

Toluene

The earlier pulls were light brown.