The Vespiary
The Hive => Tryptamine Chemistry => Topic started by: heavenadisaster on March 23, 2003, 12:26:00 AM
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SWIM botched half their yeild of a 50g a/b MHRB extraction; evidently the defat wasn't thorough enough... does anyone have any experience redissolving this in non-polar, migrating to acidic dh20, defatting, basify and attempt to recrystalize? wouth this be worthwhile and effective?
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I would suggest that the oil is good enough and to go ahead and smoke this.
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I remember once getting an oil that never solidified. It was garbage. I gave it to someone else to smoke and it was mildly psychoactive. I wasn't about to smoke mystery goo. Actually, I did a little. perhaps you overbasified.
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when SWIM thought he was up against the same problem, he was told that if it was fat, to acidify, defat, basify, etc
but also if it was too basic, backwashing might help the problem..a little dab of it on your tongue should tell you if you went too alkaline...
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ditto morbid...
swim did this (acidify, defat, basify, extract, backwash evap (slow)) and was left with nice, crunchy crystals... cleanest ever! - they should sparkle, and look wet after such treatment...
Next time, dont skimp on filtering the sediment after the initial acidic soak(s)!
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wow..SWIM must have been thinkning along the lines of SWIY... ;)
the unfortunate news here is that SWIM's extraction failed (how embarassed he must be to have fucked up an A/B)...though he tell me that there is a half a jar of gook left, just waiting for a lazy day of experiementation, he tells me...
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It may be useful to dissolve the oil in warm naphta and then chill slowly to as cold as possible. Save the crystals.
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If you used naptha, it should be fairly clean, but if you used something else, it won't be as clean
It is worth another go through the acid/defat/base/wash/extract. crystals are the result of a certain level of purity.
I have found that toluene is very good for the defatting, it rips the crap out of it totally.
And like god says, if you've cleaned it properly, it sparkles, it might be yellowish, but it will sparkle.
The water wash at the end can also be done with tapwater too, tap water is slightly alkaline and will draw up any crap in the nonpolar that is slightly soluble in water.
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used dcm for the defats and got oil on the extractions with with ether and chcl3.
swim is currently in the process of trying again, this time doing the washes... this seems to be very important.
with the current oil two conflicting suggestions have been made: redissolve in acidic water and defat, wash, basify, extract, or redissolve in np (naptha was said) and pull down the temp till crystalization. any thoughts on this issue?
swim appreciates the comments.
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swims advise comes from direct 'dreaming' experiance- although he never tried the heat-cool thing (in naphta), he has a very strong hunch that some of the oils will most definatly follow along- specially considering the fact that their mp is lower than the DMT (he knows this for certain). Swim once carried at batch of peanut-buttery crap with him to a festival... the heat from the sun melted the oils/excess -OH. It separated into 3 (not very distinct) layers with the good stuff predominantly on the bottom. Even after attempting to separate the good 'layer', once it was cooled- it was still an ugly mess. There was considerable mechanical loss ta boot (although this was not done with a sep funnel). Dont bee lazy! Do it right, it'll bee a good learning experiance as well.
No short cuts! If swiy desires clean crystals, do it the 'right' way.
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SWIM can report that recrystallising in naptha does indeed work, it can yield nice little table salt sized pure translucent crystals of dmt in about an hour after dissolving just barely in hot naptha in a closable container and then putting straight in the freezer. There seems to be a thin layer of a yellow contaminant that warm/cool cycling seems to isolate from the dmt, and further that the yellow stuff doesn't actually crystallise, it forms a resin. This, mind you, was with acacia obtusifolia, so mhrb might be a little different.
SWIM hasn't fully experimented yet, but intends to find out whether alternating the recrystallisation solution between warmer and cooler environments (room temp, fridge, freezer) progressively towards the freezer temp will eventually result in larger crystals.
The contaminants causing the extract to oil out are probably high boiling elements from the naptha, so long as the naptha isn't allowed to lose too much of the low boiling element when heating it (ie if done quickly) the much more naptha soluble crap will definitely wash off when the solvent is removed from the crystals.
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good!
it would bee interesting to see what would happen if the discarded layer contained any goods (via extraction) to see what kind of losses occured (if any significant)
Sounds like an easier, less time consuming method provided losses arent too great
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One thing that can be done with the discarded solvent is simply throw it onto a drying dish and see if any crystals form. I wouldn't think that there would be much loss, not much would dissolve in the shellite at -20°C - not much dissolves in it at room temperature.
SWIM is itching to get some IPA and use it as the recrystallising solvent rather than shellite, on account of the more uniform fractions dissolved in the solution - the shellite has a very wide fraction in it, probably between about 40 and 90 degrees.
SWIM had a nasty experience with using a pH 12 wash of the nonpolar extraction which the end result had a lot of hydroxides in it, rendering the product virtually useless. SWIM will use plain tap water in future, it gets the water soluble gunk out much better, and leaves nothing behind.
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In order to achieve greater uniformity in the crystals, I would think that it is important to do frequent temperature transitions, every half an hour, and to start with room temp/fridge/roomtemp/etc first, and then go to the fridge/freezer combo... Otherwise impurities will get trapped within crystals.