The black/crystalline powder could very well be partially anything.

The pleasant dose is difficult to find, particularly if you are working with a product batch of unknown purity.
Thus it is beneficial to know your dose.

How can I theoretically go about: further purifying/measuring out an accurate dose?

1.) recrystallise.

Minimum amount of hot solvent onto dry solid (heat solvents on a water bath), gravity filter, and let it cool slowly, if it gets down to room temperature and nothing has come out, wang it in the freezer for a day or three. If the solution that you filtered is still an ungodly colour, its activated charcoal time.

clean enough? Measure out and take, start with a low dose, work from there.

2.) Not clean enough? Probably your best bet is another recrystallisation, you could try ammonia washes or filtering with activated carbon.

If you need to use activated charcoal, use only a little, about the amount of a pea, add it to a (hot) solution of your product, and gravity filter it. Perhaps wash a little more hot solvent through the filter paper to get anything that crystallised out when it ran through the filter paper.

3.) Still not clean enough? Do another A/B on the product, use ready made up solutions of your acids and bases in distilled water, you don't want to rape your molecule and end up with a pile of gunk.

4.) Still not clean enough? Column chromatography, hardest just becuase of the bugger of getting the equipment, but generally will give you the cleanest extraction of your desired product, whilst losing the least.

5.) STILL not clean enough!? ...start again, and put this one down to a learning experience :(

All joking aside, a good recrystallisation is probably all you need, maybe start with an ice cold ammonia wash.

Can you get pictures up? There's yellowey crystals, there's mescaline HCl shards, and there's black gunk, if you have the latter, its recrystallisation for you I'm afraid.

EDIT ; If measuring an accurate dose is a problem, buy some scales. At least ones that will measure to +/-0.1g, then make up a solution, say 100ml, of your product in distilled water, and calculate your dose from there. I haven't checked to see whether mescaline will dissolve in water, so don't quote me on that.

Thank you, Van Bass

I dont have a vacuum pump.

Actually i have scales of that display to the .01 that have been calibrated with non-official, but good-enough weights.
I also have one of those relatively cheep 0.001 display scales.
Everything from temperature, to where i stand(wooden floor shifting) fluctuates the scales.:mad:

Should i, theoretically, have de-fated prior to the A/B, inorder to get the nice pure crystal sought.

How should i properly calculate the precipitation reaction?
I only know a few basic organic-chem principles and the precipitation reactions learned from general chem.
I really don't wish to have dangerous/unnecessary contaminants in my precipitation.


This is all theoretical in nature, and just out of curiosity.

Should i, theoretically, have de-fated prior to the A/B, inorder to get the nice pure crystal sought.

Yes.

Also, recrystallize in MEK, though don't be surprised if the yield is dismal. At least, that's what I found on my first try. (But I used ~1ft of cactus cut from a much larger plant. If you used more, you may be in luck.)

Do you have a WD account? Because Tramp posted a fantastic pictorial on the recrystallisation of mescaline from MEK. I would personally say to follow that if you can find it, if not just follow the basic guide I posted for a recrystallisation.

There's nothing really to be calculated in a recrystallisation, its just a bit of a skill/knack; its not even a reaction, just dissolving and playing around with solubilities at different temperatures.

Of course, should you choose to use MEK, having decent quality MEK obviously counts, although you won't be evaporating solvents, there will be residue on your product, even traces after washing I would guess, so you want it to evaporate clean!