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can naphtha be too saturated to freeze precip? Options
 
*oneironaut*
#1 Posted : 6/6/2013 2:38:21 AM

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I have a very milky jar that doesn't seem to want to crash out and is staying milky.. wondering if the solvent can be too saturated to let crystals form. Also there is a layer settling on the bottom, which I presume to be the goo with fats/oils.

Second part to this, if yes it can be too saturated then does this apply to evap also?

Thanks for any input Smile
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shanedudddy2
#2 Posted : 6/6/2013 3:13:48 AM

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My guess is that it is saturated with something else, which does not freeze precip.
Can always evap to see what you get.
Worst case is that you can re-xtal and freeze precip from there.
 
cyb
#3 Posted : 6/6/2013 8:01:44 AM

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Agree with Shane...or you could dilute with more solvent and try again in the freezer.
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*oneironaut*
#4 Posted : 6/6/2013 1:58:49 PM

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Saturated with something else? NMT? It's acbr so that could very well be, the pulls were very clean and it didn't cloud up until it cooled... I'll probably just let it evap and enjoys whatever this little gem of a plant has to offer Big grin

Thanks for the responses. But let me ask, in a perfect scenario where it was pure dmt and only solvent CAN it be OVER saturated for a crash to happen?
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Ambivalent
#5 Posted : 6/6/2013 2:13:51 PM

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my logic is that when solvent is super saturated, alkaloids will start to crash out instantly even before you get it in the freezer. because naphtha is really volatile and evaporating slowly even on room temperature, i have observed dmt starts to form a ring on the upper part of the vessel used.

so from my experience, if the solvent is super saturated, dmt will crash out sooner.
 
*oneironaut*
#6 Posted : 6/6/2013 3:59:14 PM

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Ambivalent wrote:
my logic is that when solvent is super saturated, alkaloids will start to crash out instantly even before you get it in the freezer. because naphtha is really volatile and evaporating slowly even on room temperature, i have observed dmt starts to form a ring on the upper part of the vessel used.

so from my experience, if the solvent is super saturated, dmt will crash out sooner.


this would make more sense to me. My understanding would be that if a solvent is "saturated", it means it can't hold any more alks, therefore it could never be "over saturated"

I was wondering if maybe the term saturated was being used more loosely in place of high concentration.

So Ambivalent, in your experience in the case of super saturated solvent crashing out instantly, what form did the alks drop out in? I'm assuming not crystals as this would take time to form, right?
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Ambivalent
#7 Posted : 6/6/2013 4:23:15 PM

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with my observations, the first signs is the formation of that ring of alkaloids on the vessel i mentioned previously, it usually formed where solvent was in contact with air. so im guessing how much alkaloids will drop out before you get it in the freezer really depends on the temperature and evaporation rate of the solvent and how saturated it is..

when it formed it was very porous crystal formation, almost powdery which sticked to the glass.

 
Apoc
#8 Posted : 6/6/2013 7:06:20 PM

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what naphtha are you using? I have used some naphtha sold as lighter fluid that does the same thing. I think there is more than just naphtha in it, and have lost some yields.
 
*oneironaut*
#9 Posted : 6/6/2013 8:03:26 PM

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Apoc wrote:
what naphtha are you using? I have used some naphtha sold as lighter fluid that does the same thing. I think there is more than just naphtha in it, and have lost some yields.


naphtha is good. http://www.amazon.com/Kl...tha-Quart/dp/B001G9TGQI

have used it many times and evaps clean.

So one thing i guess i didn't mention is that the jar I have that is in question was a combo of two freeze precip jars that did crystalize but somewhat melted leaving them stuck in a very sticky film, so I took some of the said nap, heated it up and redissolved both of the other jars into about 100ml poured into a new jar and discarded a small bit of yellow sediment which i assume was just oils.

Since I combined two pulls worth of spice into the same amount i did one pull with plus the fact that it was reused nap from the previous pulls led me to believe that it may have been too concentrated to crash. I have only let it sit in the freezer for about a day and a half so it may be more a matter of time.. but what is there as of this morning is a layer of off white goo and still relatively (but less) cloudy solvent. May just be a matter of time???

Does NMT behave differently during precip.. could it be that??



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Ambivalent
#10 Posted : 6/6/2013 8:58:32 PM

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my guess is that you have more "contaminants" than dmt in there. thats why it is behaving like that. why dont you just evaporate and see what you are left with, you can clean it or infuse it afterwards anyway.
 
Hiyo Quicksilver
#11 Posted : 6/6/2013 9:32:17 PM

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I've found that sometimes crystals don't like to form if there's a thick layer of sediment or precipitate on the bottom. I had good luck letting it settle then removing the solvent to a clean jar and putting it back in the freezer. I then collected that oily sediment and washed it with fumaric acid, and it was mildly potent.
 
*oneironaut*
#12 Posted : 6/7/2013 4:31:52 AM

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Ok, so came home today and nap was clear and what crashed out was a light brown/ tan colored crumbly sediment. Some of it was loose and some was pasty... drying it now. I think it must be plant oils mixed with it...I'm quite confident little to no base made it through.

I did my pulls while the jar was probably a little to hot (I had it in a near boiling waterbath) and am thinking that many have pulled more gunk along with it... I think a warm bath would have served me better than hot.. the jar was almost too hot to hold while shaking. Does my thinking seem in line with the resulting crumble (almost like brown sugar, but lighter)?

I may re-ex but what was there wasn't that much.. maybe 150mg
The rest of the pulls I did before this jar are slowly evaporating in a pirex dish. I 'm estimating it will take a couple days to evap, so wish me luck on that one Smile
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*oneironaut*
#13 Posted : 6/7/2013 4:05:55 PM

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Thanks again for your feedback guys... so final report on this.....

Moral of the story:

1) Patience is a virtue!

2) Need a lesson in eyeballing yield! It ended up being just shy of 560mg. Amazing how much bigger it looks once you get it out of the jar and spread out on a filter. The color and consistency once dried was light tan with a slight waxy texture... alllll gooooood Big grin Can't wait for the rest to evap and get a final yield.. should hopefully be around 2%, we'll see. (this jar was a combo of the last two of 5 pulls of 250g of ACBR btw)
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Hiyo Quicksilver
#14 Posted : 6/7/2013 9:33:52 PM

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Haha "junk". It's delightfully psychoactive, you know.
 
*oneironaut*
#15 Posted : 6/8/2013 12:07:17 AM

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Hiyo Quicksilver wrote:
Haha "junk". It's delightfully psychoactive, you know.


Laughing Gunk NOT Junk Wink

But i was referring to the oils and fats not the NMT or any welcomed alks. I actually like the goo as much as a pure crystals... Drool
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shanedudddy2
#16 Posted : 6/8/2013 8:14:48 AM

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have you sampled the goo? I`ve both had goo that rocked my world, and goo that did little to nothing but give me a very sore throat
 
*oneironaut*
#17 Posted : 6/8/2013 5:11:41 PM

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shanedudddy2 wrote:
have you sampled the goo? I`ve both had goo that rocked my world, and goo that did little to nothing but give me a very sore throat


The particular pull in this thread came out as a light tan brown sugars powder, which I have not yet sampled. However, I did get some goo from a test batch I did a while back that was from the same bark and it was very nice, not extremely potent but nice nonetheless. I had made changa using passion and caapi leaf...so also probably why it was a bit more mellow.

I have no doubt this "brown sugar" will rock me Smile

The rest of this batch is evaporating and should be more of the white crystals iif they form and/or the clear dmt/nmt goo (more likely)

I expect nothing but world rocking from it Very happy

You can't do anything about yesterday, but you can do everything with tomorrow.

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AuroricDistortions
#18 Posted : 6/12/2013 3:14:15 AM
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*oneironaut* wrote:

So one thing i guess i didn't mention is that the jar I have that is in question was a combo of two freeze precip jars that did crystalize but somewhat melted leaving them stuck in a very sticky film, so I took some of the said nap, heated it up and redissolved both of the other jars into about 100ml poured into a new jar and discarded a small bit of yellow sediment which i assume was just oils.

Since I combined two pulls worth of spice into the same amount i did one pull with plus the fact that it was reused nap from the previous pulls led me to believe that it may have been too concentrated to crash. I have only let it sit in the freezer for about a day and a half so it may be more a matter of time.. but what is there as of this morning is a layer of off white goo and still relatively (but less) cloudy solvent. May just be a matter of time???

Does NMT behave differently during precip.. could it be that??



I had some orange xtals from the 2nd & 3rd extractions on some acrb, reduced the used naphtha to 1/4 its original volume. Then heated the remaining naphtha to near boiling, and dissolved the orange xtals. I also had a light orange oil sediment left at the bottom, which I saved in the tray. The naphtha has been sitting for 8 hours at room temp and is slightly cloudy with very few tiny xtals formed. The orange sediment has mostly crystallized in the familiar dmt pattern and I suspect that is where most remained.

It seems that reducing the naphtha boiled off the lighter fractions,thereby concentrating the heavier fractions along with the acacia fats & oils and rendering the naphtha ineffective as a solvent? Std. A/B with acetic acid, NaOH, and MgSo4.
 
 
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