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Yellow goo. Wont crystallize Options
 
Delta-9-THC
#1 Posted : 2/7/2009 1:26:34 PM

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After evaping my first 3 pulls combined using a hot blow dryer I ended up a with a slightly gooey yellow substance that doesn't seem to want to crystallize.

I have always done 50g batches before this way and it worked fine. This time i tried doing 150 g. The naphtha was WAY more yellow than with the smaller batches.

It only has a few tiny crystals in the side. Is this from all the fats and oils or is it because I used hot air to evap? I also added the lye to fast and it got very hot for a few minutes. Any ideas what happened and what I should do?

I have one more pull (150ml naphtha) that I left in the solution overnight. Maybe I should just dissolve the goo in it and try a freeze precipitation?

I have always done 50g batches before this way and it worked fine. This time i tried doing 150 g. The naphtha was WAY more yellow than with the smaller batches.
 

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burnt
#2 Posted : 2/7/2009 1:45:15 PM

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SWIY could try a number of things. Either redissolve the goo in a small amount of naptha and rinse the naptha with basic water (sodium carbonate pH 12 or so) then crystallize the spice out the naptha. Or skip the rinsing and just try to recrystallize by freeze precipitating. This will help to remove the impurities.

There could be a number of reasons SWIY is seeing more yellow goo then usual. Ranging from the heat to the amount of bark used to the batch of bark used. It doesn't really matter though there is always a chance of that yellow stuff being there thats why recrystallizing is useful way to purify.

 
endlessness
#3 Posted : 2/7/2009 2:12:52 PM

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many times SWIM got a goo that would refuse to crystalize. Many of these times, SWIM was patient and kept scraping the goo up, and then rubbing it back again into a plate (or on the sides of the baking tray where it was evapping). Doing this over and over again once in a while for a few days would make a lot of it end up crystalizing.

and if nothing worked after a few days, SWIM redissolved it all in a small amount of warm naphtha (SWIM calculated how much he thought there was of DMT and used a ratio of 30ml warm naphtha per g of dmt) and then into the freezer
 
Delta-9-THC
#4 Posted : 2/7/2009 2:36:10 PM

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Yes tiny parts have begun to crystallize. This prompted my to put the fan on low over it. When I came back all the crystals had disappeared. This probably happened because the fan blew the goo over the crystals. I will just have to leave it. If it doesn't start to crystallize by tonite I will dissolve it all in my last pull and stick it in the freezer.
 
Delta-9-THC
#5 Posted : 2/7/2009 6:59:41 PM

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Sorry to double post but I kinda need a second opinion. I believe that the heat probably converted it to n-oxide which is apparently insoluble in naphtha and won't crystallize. It seems there is also a fair amount of NN DMT in there because a lot has crystallized. But its still slightly gummy. I believe this is from the n oxide mixed in.

My plan is to pour my last pull in the evaporation dish with the yellow goo/gum thats been drying out. Then I will have 150ml naphtha saturated with all the DMT. I will stick this in my freezer which has a temp of -5 f. The problem is the n-oxide. WIll it crystallize in a freeze precip? Or at least stay behind so it isn't lost with the solvent. What do you think is the best plan?
 
endlessness
#6 Posted : 2/7/2009 7:10:44 PM

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SWIM wouldnt mix it.

SWIM would be patient and re-scrape it for another day or two, he had success this way.

The other pull SWIM would stick in the freezer separately.

If its n-oxide, it wont crystalize and wouldnt dissolve even in warm naphtha. It is an oil and insoluble in naphtha. One could do the n-oxide conversion back to dmt using zinc dust, or just smoke it with herbs. Just dissolve it in alcohol, put some herb and let evaporate, and then smoke the herb. Also dissolving in alcohol would give more time for any residual solvent to evaporate.

The disadvantage with n-oxide with herbs is its hard to see dosage, so experience will be your scale. The trip of n-oxide in SWIM's opinion is same same as dmt, but some people say its different, maybe even better.
 
VisualDistortion
#7 Posted : 2/7/2009 10:12:27 PM

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Could you evap the solvent with a hotplate in an argon atmosphere to prevent N-oxide dmt from forming?
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DarkShaman
#8 Posted : 2/8/2009 1:13:39 AM

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2 words of advice:

Heptane recrystalization.
 
Delta-9-THC
#9 Posted : 2/8/2009 2:20:07 AM

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I dunno, at this point it seems it isn't ever gonna fully crystallize. Even the parts that have formed into crystals are still very sticky and gooey when scraped. I don't have any heptane.

I'm not really quite sure what to do. Im not sure if I should try and combine it with my last pull and freeze precip. I am tempted to do this but I'm afraid of losing the n oxide.

I also am afraid of smoking this gummy goo on the chance that it still contains naphtha, although it smells nothing like naphtha and only like DMT.

I also will have to be going away tomorrow night. If I cannot get it to crystallize, is there and way I can store it so I can finish crystallizing in about 5 days?

This extraction turned out to be a nightmare. I definitely learned a few good lessons though.
 
halcyon
#10 Posted : 2/8/2009 3:46:03 AM

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Sometimes SWIM wonders if he/she is missing some really important post about "yellow goo". It seems that yellow goo is almost ALWAYS the product of heat. SWIM has seen this a number of times before. Heating the saturated Naptha (or other solvent) will do this (even if only below 55C) - heating the basic mhrb solution in open air (ie double boiler) will also do this. SWIMs foaf has never had this problem with heating solvent the solvent before dumping it into ROOM-TEMP mhrb solution. So, in this humble observers mind the combination of heat and lots of free oxygen will create yellow goo. Apparently using zinc dust can bring it back to its normal form.

I have heard that some people here have mixed yellow goo with other intert substances so that it was easier to handle. 69ron, and other pros, can you elaborate on this?
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VisualDistortion
#11 Posted : 2/8/2009 8:18:36 AM

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That's why i ask the question of evaporating the solvent in an argon environment. The dmt couldn't oxidize no matter how hot you got it because there would be no oxygen. IDK, maybe that's getting to far out there.
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mayahuasca
#12 Posted : 2/8/2009 9:15:42 AM

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DarkShaman wrote:
2 words of advice:

Heptane recrystalization.


you got it.

use heptane.

redissolve it all in boiling heptane and all the junk will settle to the bottom and then you pour off the good stuff which is all in the heptane to another glass.

let that cool at room temperature for a few hours. then put it in the fridge for a few hours, then in the freezer for 3 days. that will really clean it up. you can still re-crystallize further if you like until you have pure white crystals.

 
endlessness
#13 Posted : 2/8/2009 12:52:19 PM

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just leave it as is for 5 days.. it wont hurt it.. Just put a soft cloth so no dust goes inside, but not too thick cloth, so that it can still 'breathe' and evaporate remaining solvent

do what you want but as I mentioned, SWIM does NOT advise to mix the pulls, its silly, in the end even if you have nice crystals from the other pull, it will drown in the oil and be mixed.. leave the pulls separate

either recrystalize (but if its n-oxide, it wont be dissolved even in hot heptane/naphtha, so it would stay together with whatever impurities

I already also mentoned, if you are affraid of smoking solvent remains, redissolve it in alcohol and then soak some herbs. This will give more time for any solvent to finish evaporating. Also you can use hot plate (not warmer than 50-60 degrees) to help further evaporation.

In SWIM's experience, even if it does not at all seem like its gonna crystalize, re-scraping it and rubbing against the wall of a plate a few times over and over for a few days will help a lot. and if not the alcohol+herbs always works, or recrystalization with hot solvent but you will lose any n-oxide this way.

and once again dont mix the other pull with this, its a bad idea
 
Delta-9-THC
#14 Posted : 2/8/2009 1:04:36 PM

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Ok, Thanks a lot endlessness. I really don't want to have to mix it with herb because I can tell I have over 1 gram in the plate. I don't wanna have that much herb/dmt mix. I am really only looking to get relatively pure DMT.

At this point, if i scraped it up it would be a gummy sticky substance. Store able, but very difficult to work with and weigh out. Also, if i scape it up it will probably never dry out any more than it has. I supposed I will have to leave it like this for a few days. I think there is minimal, if any, naphtha left in there but I can wait 5 more days just to make sure.

Well at least I get to see if n-oxide changes the effects at all.

 
endlessness
#15 Posted : 2/8/2009 1:21:51 PM

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Delta-9-THC wrote:
Ok, Thanks a lot endlessness. I really don't want to have to mix it with herb because I can tell I have over 1 gram in the plate. I don't wanna have that much herb/dmt mix. I am really only looking to get relatively pure DMT.

At this point, if i scraped it up it would be a gummy sticky substance. Store able, but very difficult to work with and weigh out. Also, if i scape it up it will probably never dry out any more than it has. I supposed I will have to leave it like this for a few days. I think there is minimal, if any, naphtha left in there but I can wait 5 more days just to make sure.

Well at least I get to see if n-oxide changes the effects at all.



SWIM already did different things in cases similar with yours. In the case of the herbs, he for example weighed a certain amount of alcohol, dissolved the goo in it, weighed again. Then he knew the weight of it. He would then make a 50/50 mix (not counting the alcohol weight obviously) with camomille (though other people use other herbs) and it was quite ok, just loading 100mg in the bong/pipe instead of 50 and it works perfect.

but if you really want to avoid this and want crystals, do a search on the 'n-oxide to dmt zinc reduction' tek, which will turn it back into normal dmt. but only if you can find elemental zinc/zinc dust/pure zinc.

there is also the possibility that it is not n-oxide, but rather just a thin film of solvent that doesnt evaporate, or some impurity/fat from the extraction. In this case, doing as people said and running hot solvent in it for a minute or two, pulling the solvent to another clean container and leaving whatever doesnt dissolve, and then sticking in the fridge would be perfect. You said you think there is over a gram of dmt there, so the amount to use of warm naphtha would be about 30-40ml...
 
Delta-9-THC
#16 Posted : 2/8/2009 1:45:42 PM

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Hmm. The real question is whether it is n-oxide or naphtha left over. It smells nothing like naphtha. Also, when exposed to heat, it begins to melt into a goo again. Any idea what that might mean?

The reason I think it is n-oxide is because of how much heat I accidently exposed it to at multiple times during the process and particularly because of the hot blow dryer which kept it from crystallizing. If there was Naphtha in there still, wouldn't the heat tend to help evaporate it?

Since n oxide is a oily goo at room temperature, and my batch may be a mix of NN/N-oxide, would it become more viscous when exposed to heat?

Edit: Update!

I Just smoked the tiniest amount and had my first entity contact!
I wont go into too much detail but heres a short description: I didn't get to see it more like sensed it, the entity held me in its arms(?) telling me everything would be OK, it also seemed to be upset when I questioned if it was real. It somehow insisted it was real but in the end it told me I must decide for myself. Beautiful.

Im pretty sure there is no naphtha left. It tasted fine and there where no ill effects at all when i vaped it.
The only problem is its very hard to work with and weigh out. Because of its gummy consistency, even what looks like a tiny amount actually weighs quite a bit.

Edit 2: Do you think that if i put it in the freezer it might harden? It starts to turns back into goo if it is exposed to heat so maybe it will do the opposite when cold.
 
DMTripper
#17 Posted : 2/9/2009 2:06:30 AM

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You can dissolve the n-oxide in isopropyl alcohol and mix it with herbs such as mint leaves 50/50 or maybe one third spice two thirds leaves.
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69ron
#18 Posted : 2/9/2009 2:22:01 AM

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DMT needs to be in contact with oxygen to form DMT N-Oxide. At room temperature it forms slowly over the course of a few years. It forms faster as the temperature rises. You can convert all your DMT to DMT N-Oxide by heating the DMT to it’s melting point and blowing a fan over it. I think something like 1 hour is all that’s needed. I’m not sure about that though. I need to check on that. I saw a tech for it a while back. Another way to make it in a matter of minutes is by dissolving DMT in a mix of 30% hydrogen peroxide and ethanol (I forget the extract ratio).

If you have mostly DMT N-Oxide, it will be slightly yellowish, will never crystallize no matter what, and it smells very much like DMT, but maybe more musty. You will NOT be able to ever freeze precipitate it in heptane, hexane, naphtha, etc., because it’s insoluble in those solvents. If you can recrystallize it, it’s not DMT N-Oxide, but just dirty DMT (the “dirt” could be DMT N-Oxide though).

If you can’t dissolve it in naphtha, heptane, or hexane, then it’s DMT N-Oxide for sure. Unless you have zinc to do an N-Oxide reduction step, you’re stuck with DMT N-Oxide.

DMT N-Oxide is a pain to use because it’s oily. It’s hard to measure out doses of it. You’ll need to either lace some herbs with it, or add something like calcium carbonate to it. Personally, I like the idea of adding calcium carbonate to it. It’s very simple. You measure out an amount of calcium carbonate, say 1 gram, then mix it in along with some acetone to dissolve all the DMT N-Oxide. Then let it evaporate. If it’s still too sticky, repeat until enough is added to make it powdery. It works really well. Just keep track of how much calcium carbonate it added. When done, weigh it out and subtract the amount of calcium carbonate you added and then you know exactly how much DMT N-Oxide you have so you then calculate your doses accurately.
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69ron
#19 Posted : 2/9/2009 2:27:06 AM

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SWIM actually like DMT N-Oxide more than DMT, but it’s a pain to use because you can’t crystallize it. SWIM has found that DMT N-Oxide is much friendlier than DMT, has a slightly slower onset, and lasts a little longer. But it’s also weaker, maybe 1/2 as potent?
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Jorkest
#20 Posted : 2/9/2009 2:40:34 AM

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what exactly is different about the effects...is it just as visual..or is it slightly dampened down
it's a sound
 
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