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How much loss to expect when washing crude mesc HCl with IPA?
- Thread starter w0mbat
- Start date
My red cat still has to try the washing of mesc using (acetone and) IPA. So he is eager to learn from your experience.
I read about some monkeys that do not have (that) much loss from IPA wash.
Was it the first time you opened the bottle of IPA?
did you use an open glass when you put it in the fridge to precipitate the solids from the IPA?
how did you remove the IPA from the solids? decant? pipette? syringe? dropper?
I read about some monkeys that do not have (that) much loss from IPA wash.
Was it the first time you opened the bottle of IPA?
did you use an open glass when you put it in the fridge to precipitate the solids from the IPA?
how did you remove the IPA from the solids? decant? pipette? syringe? dropper?
If the mescaline was a very dark colour before the wash then this sort of loss is expected.
If too much Hcl was used when salting out, it will pull a lot of crap other than mescaline which is usually the reason for such a loss in mass.
The only other thing I can think of is there was more water than expected in your IPA. Always keep your solvent washes to evap if something unexpected happens.
If too much Hcl was used when salting out, it will pull a lot of crap other than mescaline which is usually the reason for such a loss in mass.
The only other thing I can think of is there was more water than expected in your IPA. Always keep your solvent washes to evap if something unexpected happens.
w0mbat
Rising Star
My friend says he only used IPA because he wants to stick to food-grade reagents. He put about 200 mL of 91% IPA in a glass, and added way more than enough home-made "anhydrous" magnesium sulfate.* He thinks it was an excess amount because the AMS formed 2 layers in the bottom of the glass: 1 solid, clumpy layer, and 1 "dusty" layer. He then stirred the IPA-AMS solution, waited for it to settle, and then drew off only the top 20-30 mL of dried IPA.Virola78 said:
This IPA was then run through a coffee filter (to remove particles of magnesium sulfate), and then placed in a glass dish that was covered with an air-tight plastic cover. This was then placed in his freezer for about an hour. The cold IPA was then added to the ~0.6 g of crude mescaline HCl in a beaker and stirred. My friend says at this point, it seemed like almost all of the solid had dissolved (even though it was cold IPA
). This solution was then filtered through a coffee filter. After scraping off the remaining solids from the coffee filter, the filter itself was soaked in distilled water twice to remove any remaining water-soluble mescaline HCl.My friend feels that filtering the IPA & mescaline HCl through the coffee filter was a bad idea, and will not do this next time. Instead, he'll just wait for the solids to settle and then decant the IPA. BTW, what do you recommend for removing the IPA: decanting, an eyedropper, a pipette, or a syringe? Would a plastic syringe partially dissolve in the IPA?
He is nervous about trying to recrystallize Mesc. HCl from IPA, mainly because he wants to keep his technique as simple as possible so as to avoid any more screwups.
* the reason I put "anhydrous" in quotes is because the magnesium sulfate was not truly anhydrous. My friend said he started out with mag sulfate heptahydrate, and by the time he finished heating it in his oven, the weight had not decreased enough for it to be completely anhydrous. However, he still thinks his magnesium sulfate can still be an effective drying agent, even though it's probably mono or di-hydrated. (can anyone comment on this?)
w0mbat
Rising Star
Phlux- said:
My friend dried it as much as he could, so he assumes it was 99% IPA.
Phlux- said:
He would use acetone if he could acquire it in Food Grade or better quality. Do you know of any places he might be able to find this? The only way he can think of acquiring it is by distillation
w0mbat
Rising Star
soulfood said:
It was not all that dark to begin with, and it did become lighter after washing, but not all that much lighter. It also had (before and after washing) a kind of buttery consistency, almost like crude mescaline acetate
soulfood said:
He used three batches of ~20 mL of roughly 7% HCl. Is this concentration & volume what you guys use?
soulfood said:
He has kept the IPA in his freezer, and says that there's some dusty stuff floating around in it, but no crystals on the bottom per se. Would it be worth filtering this stuff out, or maybe evapping all of it and washing again with a smaller amount of IPA?
w0mbat said:
The cat has done 3 batches of 25ml 2% HCl. There were some nice crystals in the evap plates. Some looked like the fine clear crystalshards that Phlux- has produced and photographed. But there was also an orange coloured stuff present. All the stuff was easily scraped (broken) off the evap dish. (The acetates some time ago were allot more difficult to scrape off the dish.)
Anyways, the dirty mesc-HCl was washed twice with 2x 10ml acetone, using a small shotglass and a dropper. In between these washes the stuff was not left to dry. Some tan colour is washed off by the acetone, but the mainproduct is still very much tan coloured. Drying at the moment, then an IPA wash will be done.
Why is this washed product not fairly white yet? was the acetone wash not rigorous enough?
Or will the IPA wash off the remaining dirt?
Or is the pulled product just too dirty to clean up using acetone and IPA?
Silly red cat.
w0mbat said:
I've never been too much into working out the exact percentage of what I'm using, but my hcl out of the bottle is 30%. I just add literally 2 tiny drops into 20-25ml water and that's enough to bring it to the right pH.
w0mbat said:
The crystal shards were somewhat crushed and swirled in the acetone. The shotglass was left for some time to let the solids settle. The acetone didnt take on much brownish colour and was sucked off as much as possible, using a dropper, without disturbing the powder at the bottom. Another 10ml acetone was added, swirled a bit, left to settle, and then sucked off again. The powder at the bottom of the glass left to dry a bit.
The next 2x 10ml IPA washes did take away much more of the brownish colour. And also volume of the powder had reduced quite a bit by now. Therefore it was decided to not do another IPA wash.
The powder at the bottom was left to dry and cut into a powder. There is now about a gram? off white powder, slight tan. Not weighed yet, no scale.
There will be picture and so later.
Im interested to find out more about this stuff
narmz
Rising Star
I don't think IPA is food grade. Is it? I'm pretty sure it's not intended to be consumed at all. Ethanol would be food grade though. Anywho, use acetone if you're cleaning mesc hcl, lots of loss expected for sure, you're getting rid of the other alks - especially with pedro. Do you have food grade HCL? I don't know, if you're trying to stick to more safe stuff you might wanna look into carbonates, they can be cleaned with ipa from what i've heard.
^ IPA evaporates completely as far as i have understood. And indeed, the washed product is dry powder. No smell of IPA.
The acetone, and IPA used for washing crude product are lab grade. Thats fairly pure.
Lab grade chemicals are easy to purchase in the Netherlands.
The acetone, and IPA used for washing crude product are lab grade. Thats fairly pure.
Lab grade chemicals are easy to purchase in the Netherlands.
w0mbat
Rising Star
narmz said:
My friend in the USA says it can be bought in USP grade, which basically means it's free of ugly contaminants.
narmz said:
No but it seems like you can make your own reagent grade HCl by taking advantage of HCl's tendency to off-gas from solutions. I say "seems like" because I can't say with 100% certainty that nothing else off-gasses from muriatic acid as well.
narmz said:
I suspicious that mescaline carbonate may be a myth. My friend said he tried salting with liters of carbonated water and got nothing remarkable. Also, the natural flavoring in carbonated water (that may be present even if not listed on the label) my dilute the final product (assuming there even is one)