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Was he impatient?

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cosmonaut

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A friend of mine has recently completed several (4-5) naptha pulls from a gallon of basified solution (MarsTEK). This is his first attempt at DMT extraction. The naptha and solution were kept hot and rocked/shaken/swirled for about 15 minutes each pull, and probably sat around for about 45 minutes (total about 1 hour in contact with basified solution, maybe less sitting around on the latter pulls). However, before extracting, the solution was often mixed thouroughly 5 minutes before the pull was performed. At the high temperatures and pH, any emultions settled in literally 1-2 minutes max. Maybe he was still impatient and should have waited longer. Now he has about 300ml of gold naptha in a glass baking pan out in the open, attempting to evap to about 150ml before attempting freeze precip. He was careful not to get any lye sucked up in the pulls, but because pulls were performed somewhat hastily after mixing, would the naptha have minute particles of lye that were somehow suspended in it? There weren't any visible signs of this that he could tell. Is the naptha usually gold colored after pulls? It went in clear. Does this mean he'll get yellow crystals that will need a good wash? Any tips or words of advice welcomed...peace. Pictures after 10 hours freezer, 1 hour room temp, 4 hours fridge. Going back in freezer for 24-48 hours now. The gold naptha on top makes everything look yellow. [img:c62a376be1]http://img2.freeimagehosting.net/uploads/374988cae5.jpg[/img:c62a376be1] Picture from below. You can see that without the naptha layer above coloring them, some of the crystal apprear relatively white. You can see the dark yellow blobs in contrast. [img:c62a376be1]http://img2.freeimagehosting.net/uploads/14853db379.jpg[/img:c62a376be1] [img:c62a376be1]http://img2.freeimagehosting.net/uploads/fe9be4d4e5.jpg[/img:c62a376be1]
 
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Naptha has evaped a bit, and is getting close. My friend noted the presence of little "globs" that have stuck themselves to the bottom of the pan, and on the sides to some degree. They are about the same color as the naptha solution itself (ones on bottom look slightly more "golden", but another consistancy. Is this the precursor of dmt coming out of the solution, or is this contamination? He tilted the pan, naptha ran to one corner and globs remain. He could wipe them up and get rid of them if it's contamination but he's not sure.
 
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[code:1:1c04a243fb] or is this contamination?[/code:1:1c04a243fb] It's much more probably some lye+MH. Pour slowly you naphta in another jar. When the DMT concentration is low in naphta (read clear liquid, not gold), my friend freeze the jar and the dark globs freeze while the naphta remain liquid. Then he can pour out the good naphta before evaporating it. But in your case, this would form crystals which could mess with the globs... not good.
 
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Ek, he went ahead and put the solution in the freezer for 10 hours, woke up, and there is a massive layer of yellow/ white crystals on the bottom. In the spots where the globs were though there is a very distint opaque yellow area. He's gonna let it sit out for about 30 mins, refridge for like an hour then back into the freezer maybe? Will recrystalizing help take care of this yellow goo? Maybe I can scrape up the "not-so-much-contaminated" crystals and recrystalize them separately from this yellow goo? I suspect that the high temperature during the non-polar extraction contributed to the naptha taking up a good quantity of this yellow oil. It will be dealt with...one way or another.
 
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[quote:795017fdbd]In the spots where the globs were though there is a very distint opaque yellow area.[/quote:795017fdbd] Ah well, it all depends if we are speaking about a dark-brown-purple glob coming from the original soup ot a orange-yellow opaque glob which is a smokable stuff in itself (not DMT but strong stuff). Indeed, heating the soup makes the naphta to gather more yellow...
 
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Hello Cosmonaut :D If you've got time, I'd suggest letting that jar come up to room temperature, then sticking it in a hot water bath.Stir it gently and your crystals will go back into solution, and if you've got any B solution contamination it will be obvious as a little bubble of liquid at the bottom of the jar.If you have then your best option- unless you can live with that- is to mix up some strong sodium carbonate(washing soda) solution, 'wash' your solvent with that and then reseperate and freeze precip again.
 
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That sounds like a good idea. Anyone know where one might come across a modest portion of soda ash, and what brand name it might be found at in common hardwares stores? I'll probably go ahead and let the goodies freeze for a day or two, pour off solvent, let crystals dry, and see what I end up with. Then I can recrystalize, and if it is needed I could still perform a soda wash at that point right? Would an ammonia wash likely take care of this too? ADDED PICTURES TO FIRST POST
 
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Added some bigger pictures. No pretty crystals (Evaped for few hours down to half volume, then straight into freezer. Solute must have dropped out of solution very quickly), but theres going to be alot of material to work with in the recrystalization. He'll be sure to do the cooling nice and gradually then. I think this stuff might be ok after ammonia wash/recrystalization? Dark yellow will be worked with separately from the off white. Hopefully most of the darkness will dissolve away in the wash though?
 
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Forget about the ammonia wash. There was already a discussion here about it and it is not a convincing practice. [quote:47fe03b40b]Hopefully most of the darkness will dissolve away in the wash though?[/quote:47fe03b40b] No, you must find a way to discard theses dark spots which are definitivly a residue of lye soup. My friend would redisolve the yellow spice with a bit of naphta (heated in a water bath) and slowly pour the naphta in another smaller jar avoiding the dark to go with.
 
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oooh noes! Well it shouldn't be too difficult to do at this point. Could I just put the pan as-is into a water bath and try to dissove without adding additional naptha? I'll prob end up adding a little anyway and just evap a bit while it cools.
 
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My friend says he heated the naptha and crystals disolved, a layer of yellow oil remained behind after naptha was decanted. Now that the naptha has cooled it seems to be making the yellow oily spots in the new container as well. Shout he continue this process until no more oily residue deposits itself? The naptha is still piss yellow. Am I losing large amounts of DMT in that oil, or is it probably pure bad stuff? Also, this yellow oil collected in the next container as the naptha cooled from the heating. It has been retransfered again. [img:31930c0e01]http://img2.freeimagehosting.net/uploads/cd585e72f7.jpg[/img:31930c0e01]
 
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Is that from acacia? Did you defat at all? If you have some of the basified water in there it has to go; and you will need to do repeated free precipitations to get rid of the oil. Strongly suggest you defat more before basing next time.
 
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See...!? All this fuss from STB's ! Contamination, washing, redissolving ... this tek is frought with pitfalls for the newbie who doesn't even want to know how the chemistry works. Solubilize the dmt in acidified water first. That is how you "get it" all out of the MHRB. Then filter the acid extract, and only a tiny bit of lye-solution is needed to make dmt-freebase that will run for the naphtha. This is almost fail-proof and yeild will depend mostly (only?) on the quality of the MHRB - not on all the fiddling around you have to do to 'wash' and dry the product.
 
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Ha ha ha, Elka, I wondered how much time it would take before you interact ;) Well, Cosmonaut spoke about "MasTek" which I guess is Marsofold tek. Is'nt it the 'basic' A/B tek ? Cosmonaut, The yellow is not a big problem. It may include some DMT. Let it dry completly to see if it make yellow crystalls.
 
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Yea, it was an A/B extraction, although he deviated from the tek and heated he basified solution in a water bath during the naptha pull (bad call). I'm guessing this helped force unwanted plant tannins into the naptha (He also used probably twice as much lye as I needed to). It was his first attempt, so he's working out some kinks along the way. That's why he saved over half his bark for the next pull =D. However, after transfering the naptha 3 times during the evap, there didn't seem to be any more of this oil collecting. He put it in the freezer last night, and so far he has reported nice crystals forming without all the yellow spots like before. The crystals themselves look cleaner as well. He's excited! He noted that he is having trouble restaining himself from taking it out early. I'll post pics of the baking pan for comparison when he take it out tommorrow.
 
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Yes Mars' tek is an A-B extraction, I do believe (What was I thinking !..) Maybe I jumped to conclusions after seeing those pics... ?!.. Tilt the tray around in a slow evap', to pool the oils . It seems like you de-fatted in the first pull. But yellow spice is good too.
 
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Yea, he saved one of the containers in which the yellow oil was collected, and after drying over night, theres yellow crystal structures all over the bottom. He'll have to recrystalize that stuff and see if he can clean it up a little. He said he regrets throwing out the first pool of yellow oil, lol. The stuff in the freezer is coming along nicely, pure white crystal goodness. Power went out for 2 hours a while ago, so I'm getting a C-F-C cycle going without really trying, lol.
 
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others reportedly have gotten similar results to the extraction talked about in this thread with regards to transferring the solution during evaporation. While no subjects during these reports had pools of oil as large as the pictures shown - lye/h20 impurities along with extreme oil impurities have been removed with ease using turkey basters to transfer the solvent to other containers - leaving the impurities behind. :)
 
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