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mescaline sulfate - questions

doubledog said:
Ime best way to purify is re-x of mescaline sulfate. It's really easy procedure, acetone is best for that, but IPA could be used also, it's quite similar.
During backsalting, only small amount of acid is neeed, and any excess is washed out during re-x with acetone or isopropanol.
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so cleaning mescaline sulfate using anhydrous acetone is really as simple as just putting the crystals in the acetone solution, letting the crystal precipitate to the bottom, and then pouring off the acetone?
 
it's little bit more complicated.
Dissolve your crude sulfate in very small amount of water, add small amount of acetone while solution is still warm and let slowly cool. Then put it into the fridge and then into freezer.
How nice your crystals forms depends on amount of water to acetone and how slowly it cools.
 
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doubledog said:
it's little bit more complicated.
Dissolve your crude sulfate in very small amount of water, add small amount of acetone while solution is still warm and let slowly cool. Then put it into the fridge and then into freezer.
How nice your crystals forms depends on amount of water to acetone and how slowly it cools.
Click to expand...
Yes, the role of the acetone is to reduce the solubility of the mesc sulfate that little bit more, increasing the yield, but adding too much will lead to smaller crystals. These hold on to more impurities because of their larger total surface area.

@doubledog - have you ever tried 'Ostwald ripening', whereby crystal size can be increase through careful temperature cycling? I could see that this might have an application were one to accidentally add too much acetone, or after a too rapid initial cooling.

Do we have figures for good sulfate:water:acetone ratios?
 
I prefer two step re-x, because my lazy method produces quite inpure product after salting out.

First step is precipitation from water/IPA: crude sulfate is dissolved in water (1g/10 ml) and while still warm, 20 ml or even more of IPA is added. This causes quick crystalization/precipitation - crystals are not super nice, but it is still not just amorphous material, something in between.
Liquid is decanted and product is again dissolved in warm water (1g/12ml) and then 10 ml of acetone is added, solution should turn little bit cloudy, but not milky. If it turns milky, crystalization will be too fast. Slowly cool it in fridge, very nice crystals should form. Then put it in the freezer for 48 hours. If crystals are not nice (small grains instead of longer needles) when in fridge stage, warm it again and add very small amount of water (0,5ml) and dissolve it again fully. Repeat cooling. Filter out and wash with cold acetone and dry.
Collect all liquids and washing, evaporate it and add residue into first step together with new crude product from another extraction.

It seems quite complicated, but I love the specific shining of mescaline sulfate.
Ratios needs to be slightly changed sometimes, it does not work the same all the time.

Tartrate of mescaline behaves very similarly in both solutions, but crystals are not that beautiful.

Once I have tried to grow big single crystal by switching temperatures (cool-freeze-cool-RT and so on) and it works quite good, you just need time. To forget it in the freezer for 2 weeks works also great. ;)
 
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Doubledog, if not done already, are you going to try cielo one day? I think you may like the xtlas that grow in EA over a day or so. Can be different each time.

Xtalization is such a beautiful thing. Balance of energy and forces that grow into a beautiful structure. We live in an amazing world ❤️
 
doubledog said:
it's little bit more complicated.
Dissolve your crude sulfate in very small amount of water, add small amount of acetone while solution is still warm and let slowly cool. Then put it into the fridge and then into freezer.
How nice your crystals forms depends on amount of water to acetone and how slowly it cools
Click to expand...

doubledog said:
I prefer two step re-x, because my lazy method produces quite inpure product after salting out.

First step is precipitation from water/IPA: crude sulfate is dissolved in water (1g/10 ml) and while still warm, 20 ml or even more of IPA is added. This causes quick crystalization/precipitation - crystals are not super nice, but it is still not just amorphous material, something in between.
Liquid is decanted and product is again dissolved in warm water (1g/12ml) and then 10 ml of acetone is added, solution should turn little bit cloudy, but not milky. If it turns milky, crystalization will be too fast. Slowly cool it in fridge, very nice crystals should form. Then put it in the freezer for 48 hours. If crystals are not nice (small grains instead of longer needles) when in fridge stage, warm it again and add very small amount of water (0,5ml) and dissolve it again fully. Repeat cooling. Filter out and wash with cold acetone and dry.
Collect all liquids and washing, evaporate it and add residue into first step together with new crude product from another extraction.

It seems quite complicated, but I love the specific shining of mescaline sulfate.
Ratios needs to be slightly changed sometimes, it does not work the same all the time.

Tartrate of mescaline behaves very similarly in both solutions, but crystals are not that beautiful.

Once I have tried to grow big single crystal by switching temperatures (cool-freeze-cool-RT and so on) and it works quite good, you just need time. To forget it in the freezer for 2 weeks works also great. ;)
Click to expand...
This is really helpful @doubledog! So a 1gram mescaline to 10ml water is the ideal ratio - then add 20ml IPA... Then a 1gram/12ml of water ratio and then 10ml. of acetone? Obviously every thing would be scaled up.

Was this determined through Stoichiometry or just running some experiments yourself?
 
I just did few experiments and found out this ratios. I would not say that these are ideal, it just works for me. Scaling up is always tricky, maybe some changes are needed.
But it's very forgiving procedure, if you are not satisfied with the results, just evaporate it and start again with different amount of water or acetone.
 
doubledog said:
I prefer two step re-x, because my lazy method produces quite inpure product after salting out.

First step is precipitation from water/IPA: crude sulfate is dissolved in water (1g/10 ml) and while still warm, 20 ml or even more of IPA is added. This causes quick crystalization/precipitation - crystals are not super nice, but it is still not just amorphous material, something in between.
Liquid is decanted and product is again dissolved in warm water (1g/12ml) and then 10 ml of acetone is added, solution should turn little bit cloudy, but not milky. If it turns milky, crystalization will be too fast. Slowly cool it in fridge, very nice crystals should form. Then put it in the freezer for 48 hours. If crystals are not nice (small grains instead of longer needles) when in fridge stage, warm it again and add very small amount of water (0,5ml) and dissolve it again fully. Repeat cooling. Filter out and wash with cold acetone and dry.
Collect all liquids and washing, evaporate it and add residue into first step together with new crude product from another extraction.

It seems quite complicated, but I love the specific shining of mescaline sulfate.
Ratios needs to be slightly changed sometimes, it does not work the same all the time.

Tartrate of mescaline behaves very similarly in both solutions, but crystals are not that beautiful.

Once I have tried to grow big single crystal by switching temperatures (cool-freeze-cool-RT and so on) and it works quite good, you just need time. To forget it in the freezer for 2 weeks works also great. ;)
Click to expand...
This is the way. Sulfate dilution of 0.75g to 1.0g per 10ml water seems ideal. Ratios of 4 to 5 : 1 IPA(91%) to water also seem ideal. If the sulfate water solution is sufficiently warm, i.e. 85 to 95 deg C before IPA addition, crystal formation can be sufficiently delayed to produce perfectly clear crystal. Waiting until completely cool before transferring to refrigerator / freezer results in larger / cleaner crystals. One or two crystallizations with 4:1 ratio result in perfectly clear crystals and allows for storage in the freezer without producing ice crystals. Really no need to mess around with acetone.
 
I agree, temperature is another variable to play with, and use of IPA allows higher temperatures. One can not add acetone to hot water - acetone will boil as its boiling point is quite low. We don't want that.
 
doubledog said:
I agree, temperature is another variable to play with, and use of IPA allows higher temperatures. One can not add acetone to hot water - acetone will boil as its boiling point is quite low. We don't want that.
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Of course, MEK has virually the same BP as IPA (and ethanol, for that matter). This almost brings us back round to EA, which again falls in that same narrow band of BP. Idle musings over a cup of tea, don't mind me :LOL:

Partly the point is that there may be several options for mixed-solvent crystallisations.
 
Well, with aqueous solution they'd be usable up to their solubility limits, which is admittedly pretty low in the case of EA. More generally, mixed solvents along with temperature differentials are applied for recrystallisation of a wide variety of substances. Aqueous ethanol is a classic in this respect, having much more solvent power for non-polar substances at higher temperatures.
 
Recrystallizing from boiling ethanol 95% is another simple option. Why bother with stinky/impure hardware store solvents for final crystallization? Acetone and MEK can certainly be distilled to ensure purity, but seems rather circuitous compared to the alternatives. Even the purest crystal will still trap some solvent, why not use the least toxic solvent system e.g. pharmaceutical grade ipa & h2o or food grade etoh?
 
tribo said:
Recrystallizing from boiling ethanol 95% is another simple option. Why bother with stinky/impure hardware store solvents for final crystallization? Acetone and MEK can certainly be distilled to ensure purity, but seems rather circuitous compared to the alternatives. Even the purest crystal will still trap some solvent, why not use the least toxic solvent system e.g. pharmaceutical grade ipa & h2o or food grade etoh?
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Ethanol is much more environmentally friendly. And very easy to achieve.

I read somewhere that IPA vapors are toxic. Why not use ethanol?

What proportions of sulfate:water:EtOH would you consider? and the temperature of the ethanol??
 
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tribo said:
Recrystallizing from boiling ethanol 95% is another simple option. Why bother with stinky/impure hardware store solvents for final crystallization? Acetone and MEK can certainly be distilled to ensure purity, but seems rather circuitous compared to the alternatives. Even the purest crystal will still trap some solvent, why not use the least toxic solvent system e.g. pharmaceutical grade ipa & h2o or food grade etoh?
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Are you sure that the purest crystal will trap solvent?

I think the solvent can complete evaporate cleanly if it has that character.

So, for example limonene could be problematic (?), but IPA or EA should evap cleanly away from xtals.
 
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