Pedro extraction problem

[davetheman420]

A friend of mine has been in the process of an a/b extraction. On one of the larger batches there was accidentally some lye mixed into the water/alkaloid mixture that was sitting out to exaporate. This was neutralized but whenn it exaporated he was left with the mescaline crystals that were covered in table salt. So with this being about 50% mesaline and 50% salt he was looking forr the easiest method to sepparate the 2.

Any suggestions would be great seeing that he has tried many things.

[EmmisonJ]

to quote myself:

re-a/b your product. take all your salts and dissolve them in distilled h2o, add NaOH slowly, give it a few min's to dissolve and check your pH until it has reached 12. when the pH is 12 then 99% of your mescaline hcl should fall out as mescaline freebase. add your nonpolar solvent and your mescaline freebase should move over to the np layer while the NaCl stays in the water. separate the np from the water and re-salt it. separate the np from the acid water, evap your acid water and there you go

[bucketfollower]

Glad some people actually know what they're doing lol. Good explanation man

Originally Posted by EmmisonJ

to quote myself:

re-a/b your product. take all your salts and dissolve them in distilled h2o, add NaOH slowly, give it a few min's to dissolve and check your pH until it has reached 12. when the pH is 12 then 99% of your mescaline hcl should fall out as mescaline freebase. add your nonpolar solvent and your mescaline freebase should move over to the np layer while the NaCl stays in the water. separate the np from the water and re-salt it. separate the np from the acid water, evap your acid water and there you go

[duaut]

Originally Posted by EmmisonJ

to quote myself:

re-a/b your product. take all your salts and dissolve them in distilled h2o, add NaOH slowly, give it a few min's to dissolve and check your pH until it has reached 12. when the pH is 12 then 99% of your mescaline hcl should fall out as mescaline freebase. add your nonpolar solvent and your mescaline freebase should move over to the np layer while the NaCl stays in the water. separate the np from the water and re-salt it. separate the np from the acid water, evap your acid water and there you go

Not correct. Mescaline will not fall out as a freebase.

what happens is that the mescaline will rise to the surface of the NaOH solution as a tan freebase oil.

You need to re A/B you dirty mescaline. Dissolve it in acidic H2O ph=3,and then take your premixed NaOH solution and slowly add it little by little to the acidic mescaline water and stir soon you will see the mescaline as a layer of tan or brown oil on the surface of the basic mescaline water. add a little more NaOH solution just to be sure all the mesc has separated from the basic H2O.
Then start your HCL salting over.
if done correctly this has the advantage of cleaning up your mesc to a purer product.
Never use more than 3ml of 33% HCL per gallon of Distilled H20 for salting. This will give you white Mesc HCL.
as to the pH of the basic solution, it does not matter because once the mesc rises to the surface as an oil you are ready to go to the next step.

[EmmisonJ]

Originally Posted by duaut

Not correct. Mescaline will not fall out as a freebase.

what happens is that the mescaline will rise to the surface of the NaOH solution as a tan freebase oil.

You need to re A/B you dirty mescaline. Dissolve it in acidic H2O ph=3,and then take your premixed NaOH solution and slowly add it little by little to the acidic mescaline water and stir soon you will see the mescaline as a layer of tan or brown oil on the surface of the basic mescaline water. add a little more NaOH solution just to be sure all the mesc has separated from the basic H2O.
Then start your HCL salting over.
if done correctly this has the advantage of cleaning up your mesc to a purer product.
Never use more than 3ml of 33% HCL per gallon of Distilled H20 for salting. This will give you white Mesc HCL.
as to the pH of the basic solution, it does not matter because once the mesc rises to the surface as an oil you are ready to go to the next step.

good input my friend. i assumed the mescaline freebase would fall out to the bottom as a heavier oil, sinking in the water due to it having 1.7x the density of water. not taking into consideration that the density of the water would be increased due to some saturation with the NaOH (and also in this case NaCl) dissolved in it.

i do have a couple questions for you though: why acidify the water first, why not start with neutral water? also why use a premixed NaOH solution, why not just add the NaOH until the pH shoots up to the desired 11.56+, mescaline's a tough molecule it can handle it. thanks man

[davetheman420]

OK OK. he hadn't thought of that. he don't see why it wouldn't work without acidifying the water first. He could be wrong though...
He might try it both ways and see which works best.
Its sulfate by the way.

Thanks 4 the reply's.

[EmmisonJ]

that changes things if you have mescaline sulfate, not mescaline hcl. you'll have Na2SO4 in there instead of NaCl but that's beside the point. mescaline sulfate is not very soluble in water, in fact the recrystallization solvent of choice for mescaline sulfate is water. mescaline hcl will dissolve in water with no problem at room temp, sulfate may require warm to hot water to get it to dissolve properly. swim has never made mescaline sulfate so he is not speaking from experience here. but it will crash out of the water at lower temps which may make it hard to add the NaOH. as you probably know, adding NaOH to hot water is not a good idea as it creates an exothermic reaction so be sure to keep it from boiling as it can start to boil vigorously if you're not very slow with the addition. i would say follow duaute's advice of having a premixed NaOH solution so that it's not as exothermic (should he also then chill it before adding it?) but i'm out of my element with sulfate so take my advice here lightly, i'm more 'throwing out ideas' than recommending you actually do this.

hopefully someone who has experience with the sulfate salt will chime in

[davetheman420]

Yea, he has had more problems than he'd hoped for with the sulfate.
Perhaps someone might have a bit of knowledge on the next problem too...
With using H2SO4 you have to neutralize the water before it will crystalize. By using amonia for this you also have a salty byproduct. Is this normal? How can this be purified? Would doing an acetone wash on it help anything?

[duaut]

The reason to acidify is to release any dirty molecules from the mesc.
It's the way I was taught how to clean mesc.
I've tried it with non acidic distilled H20, but the final product was not as clean as using acidic H20 at the start of a re A/B extraction.
To answer about the premixed NaOH...this is to avoid the endothermic reaction not exothermic, that happen when adding NaOH to water. possible boil over and eruptions by n00bs who may add to much NaOH accidentally.

Originally Posted by EmmisonJ

good input my friend. i assumed the mescaline freebase would fall out to the bottom as a heavier oil, sinking in the water due to it having 1.7x the density of water. not taking into consideration that the density of the water would be increased due to some saturation with the NaOH (and also in this case NaCl) dissolved in it.

i do have a couple questions for you though: why acidify the water first, why not start with neutral water? also why use a premixed NaOH solution, why not just add the NaOH until the pH shoots up to the desired 11.56+, mescaline's a tough molecule it can handle it. thanks man

[duaut]

Originally Posted by davetheman420

Yea, he has had more problems than he'd hoped for with the sulfate.
Perhaps someone might have a bit of knowledge on the next problem too...
With using H2SO4 you have to neutralize the water before it will crystalize. By using amonia for this you also have a salty byproduct. Is this normal? How can this be purified? Would doing an acetone wash on it help anything?

Titration method is needed to work with H2SO4 and is not recommended unless you can do it correctly. You just found out the hard way. Your pH was to high and you most likely lost product. Plus you need more mesc sulfate than mesc HCL to get off. H2SO4 is not a way to go for n00bs. It's a pain in the ass and not easy, yeah the crystals are nicer, but one can grow nice clusters of HCL crystals with paitence. ammonia is not recomended to create sulfate or HCL crystals. NaOH is the only way to go.