so I posted earlier about an extraction question, and wound up learning from endlessness that you don't actually have to freeze precipitate to precipitate crystals, and that you can actually just slowly evap to get your crystals.
This is mind blowing, but a few questions : I'm actually kind of annoyed when trying to get my crystals after pouring the solvent off after the freezer and find that it's not always a cut and dry procedure -.- I have bungled this a few times and it annoys me. Can someone tell me how to retrieve my crystals without the annoying part of trying to dry your crystals and get them cleanly away from ALL the solvent after freeze precipitating? I know nothing about this process and didn't even know it was possible until a day ago.
Also, what is the difference in appearance an otherwise between freeze precipitated and non freeze precipitated crystals?
Thanks nexians
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demetrispeaks wrote:so I posted earlier about an extraction question, and wound up learning from endlessness that you don't actually have to freeze precipitate to precipitate crystals, and that you can actually just slowly evap to get your crystals.
This is mind blowing, but a few questions : I'm actually kind of annoyed when trying to get my crystals after pouring the solvent off after the freezer and find that it's not always a cut and dry procedure -.- I have bungled this a few times and it annoys me. Can someone tell me how to retrieve my crystals without the annoying part of trying to dry your crystals and get them cleanly away from ALL the solvent after freeze precipitating? I know nothing about this process and didn't even know it was possible until a day ago.
Also, what is the difference in appearance an otherwise between freeze precipitated and non freeze precipitated crystals?
Thanks nexians Why did you start another thread? I did answer your question on the difference in appearance in that thread. Freeze precip can sometimes be whiter do to less oxidation, but that's not a hard fast rule. After the freeze precip you pour the solvent into another container. At this point you turn the container upside down and let it dry out, personally I find it works best if I let it slowly get back to temperature to avoid condensation, so I put it in the fridge for an hour, then upside down on some tin foil but propped up by something to allow airflow, with a towel covering it so the temperature changes slowly. After probably 12-14 hours the crystals should be completely dry and there should be no naphtha smell, at this point you can take a glass scraping blade or a razor blade and scrape the white crystals out of the dish. If you are trying to speed the process up you could use a fan, but you may get more dust particles and more oxidation. I'm really not sure whats annoying about the process, its just a few minute procedures followed by waiting.
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You must read the thread under this about residual naphtha and freeze precipitation, as I'm having a very similar issue and created the thread because of it. Waiting on the knowledgeable ones to help me out. However, I have done quite a few cut and dry, simple evaporations now and one bungled freeze precip.
The difference to me is that the freeze precip'd product was cleaner looking than the evaporated product. The evaporated stuff was a good bit more yellow and sticky or oily due to some oxidation, but still very very active. Basically if you read that thread you'll see that when I freeze precip'd I ended up with a slight off white flakey powder. When I've just evaporated it's always been a more sticky, yellow product and I've heard many others say the same thing. Keep in mind this is only after extraction with no recrystallization.
So far straight evaporation seems to be the fastest way to end up with final product for me, although I must be doing something wrong during the freeze precip. I have an idea at the end of my other post that could solve my issue with freeze precip but I won't know until someone with more experience replies.
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Hurrying is not really my concern , I'm prepared to do things thoroughly.
So to clarify, if I'm using a Pyrex baking dish, after freeze precip I pour off the solvent into another container, then refrigerate said baking dish to allow for temperature adjustment, and then turn the dish upside down on tinfoil allowing for airflow? the crystals will still stick to the dish? I'm sorry for being laborious and making another thread but I'm the type of person who does things right, but I need everything to be spelled out for me :/ the simplest things elude me
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demetrispeaks wrote:Hurrying is not really my concern , I'm prepared to do things thoroughly.
So to clarify, if I'm using a Pyrex baking dish, after freeze precip I pour off the solvent into another container, then refrigerate said baking dish to allow for temperature adjustment, and then turn the dish upside down on tinfoil allowing for airflow? the crystals will still stick to the dish? I'm sorry for being laborious and making another thread but I'm the type of person who does things right, but I need everything to be spelled out for me :/ the simplest things elude me Basically yes, the tinfoil will just help catch any naphtha that falls so its not ruining your counter tops or whatever, and any crystals will be pretty obvious if they do fall, although most will be stuck to pyrex from what i've observed. You'll want to prop the dish up a bit, like a tent on the edge so airflow can get to it. I've explained it on this thread probably with a bit more detail. https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=34633
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Thank you very much for the help, it is appreciated. I'll prowl that thread when I get home
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hey seeker, i did your method and this is what awaited me  demetrispeaks attached the following image(s):  evap 2.JPG (3,365kb) downloaded 95 time(s).
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I also had trouble getting completely solvent free crystals. What I found that worked alright was to take the container with the slightly solventy crystals and warm it just enough so that the crystals melt and you get an oily slightly yellow dmt liquid. I kept it warmed and liquid for about fifteen minutes. Then let cool to room temp. After an hour or so they were nice dry crystals.
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