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OfflineE Tard
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Registered: 11/27/99
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freeze precipitation problems - too much naptha?
    #9124116 - 10/23/08 10:23 PM (15 years, 4 months ago)

hey all.  after separating the naptha from the solution of NaOH/H20, the jar was placed in the freezer for about 8-9 hours and there was no crystal formation.  the naptha was then evaporated and there was plenty in the dish.  ~300 mL of naptha was being used.  is this too much?  would it be wiser to allow some to evaporate, then put it in the jar and freeze precip? over half of a gallon of naptha has been used in the extraction so far and only about half of the original kilo (if that) has been processed.  There is no way that this much is necessary.  The freezer seems to be cold enough according the others' reports. Does it simply need to sit in there longer?

Also, if the crystals are rather oily (feels slightly wet/sticky through the bag they are in), does this mean they have not been dried long enough?  Should they be redissolved in naptha and evaporated again, or would it be possible to just let them air dry as if they were never collected?

thanks for any feedback


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OfflineInnoculus
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Re: freeze precipitation problems - too much naptha? [Re: E Tard]
    #9124220 - 10/23/08 10:41 PM (15 years, 4 months ago)

Funny how you never said what you're extracting.  Assuming it's DMT.

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OfflineE Tard
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Re: freeze precipitation problems - too much naptha? [Re: Innoculus]
    #9124341 - 10/23/08 11:02 PM (15 years, 4 months ago)

hmm...it does seem like forgot to mention that vital piece of information.  however, i certainly thought it hard enough - maybe your telepathy unit is broken.  yes, it is dmt from mimosa


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InvisibleEntropymancer
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Re: freeze precipitation problems - too much naptha? [Re: E Tard]
    #9124396 - 10/23/08 11:15 PM (15 years, 4 months ago)

Yes, 300 mL could easily be too much. How much DMT is there when you evaporate?

The DMT being oily is probably not a result of it not being dry enough (unless it still smells like naphtha). DMT has a low melting point in the first place, so any little impurities can easily lower the melting point to where it's oily at room temp.

I'd recommend a recrystallization to make it easier to work with. Noman goes over the basics in her DMT for the Masses tek (near the end), and Entheogenist has provided a more detailed explanation/tutorial in his DMT Recrystallization tek.

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OfflineE Tard
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Registered: 11/27/99
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Re: freeze precipitation problems - too much naptha? [Re: Entropymancer]
    #9124501 - 10/23/08 11:40 PM (15 years, 4 months ago)

i dont have a scale to weigh such small amounts so its difficult to estimate how much there is after each pull...in fact i dont even know how id try and give a accurate guess at all.  there are just hundreds of tiny 'bumps' along on the bottom of the evaporation tray.  enough for quite a few doses, but that still doesnt give any sort of valid estimate being that the dosage is so variable. 

assuming that the amount of naptha is too much...would it be wiser to use less with each pull, or evaporate some of it off before freezing?  my guess is goign to be cutting back as there is a rather deep pool of naptha in the tray before evaporation and only a small layer of crystals left afterwards.  my guess is im using way too much solvent, but if that were the case wouldnt it just extract more with less pulls as opposed to using less naptha with more extractions?


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InvisibleEntropymancer
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Re: freeze precipitation problems - too much naptha? [Re: E Tard]
    #9124547 - 10/23/08 11:51 PM (15 years, 4 months ago)

Quote:

E Tard said:
assuming that the amount of naptha is too much...would it be wiser to use less with each pull, or evaporate some of it off before freezing?




Yep, if your naphtha isn't getting saturated enough for the DMT to precipitate out, definitely use less.  In general I recommend erring on the side of too little solvent per pull instead of too much, and just keep doing pulls until no more spice is coming out.  That way you don't waste solvent evaporating it (just freeze-precipitate until the last pull or two, when it's not saturated enough and you have to evaporate some/all of it to get the spice out).

Quote:

E Tard said:my guess is im using way too much solvent, but if that were the case wouldnt it just extract more with less pulls as opposed to using less naptha with more extractions?




Not necessarily; unless you're mixing the phases really well (which I don't recommend, since it can cause emulsions) and/or you're allowing several hours for the spice to migrate into the solvent, then your naphtha isn't necessarily picking up as much DMT as it could. With a smaller volume of solvent, it takes less time for the spice to migrate into the naphtha and saturate it as best as it can.

It may take a couple more pulls if you use less solvent, but you're still going to be using less solvent overall. Patience is a virtue.

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OfflineE Tard
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Re: freeze precipitation problems - too much naptha? [Re: E Tard]
    #9124587 - 10/24/08 12:04 AM (15 years, 4 months ago)

i just removed my latest jar from the freezer and here is the result.

i was using 9 oz jelly jars but while one was in the freezer (the previous attempt that initiated this post) i did two mroe pulls and placed them in a 16 oz bottle which filled it.  that was in the freezer for 9 hours.  when removed it had a couple little crystals floating around but not a significant amount at all.  after i poured it through a funnel into the collection jar, more crystals seemed to form.  i know this one may be a time factor since i used a larger jar it may have taken more time to freeze.

i just dumped it all into the evaporating dish and i guess im going to have to let it evaporate.  the extractions are going fine, so there has to be a crucial step im screwing up wtih the freezing.  does it help to evaporate some before the freezing?  if this is the case, should i just use less naptha in the initial extraction?  the only qualm i see with that is regardless of the amount of naptha used, there's still dmt left in the basic mixture so the extraction yield per pull should be proportionate to the amount of solvent used each time.

any ideas where im going wrong?  one thing i just thought of is that maybe im not allowing the naptha to mix with the NaOH/H2O enough.  maybe some additional stirring will help saturate the naptha, and therefore eliminate the need to evaporate some of it off before i freeze it?


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OfflineE Tard
Space Cowboy
Registered: 11/27/99
Posts: 1,276
Last seen: 13 years, 3 months
Re: freeze precipitation problems - too much naptha? [Re: E Tard]
    #9124591 - 10/24/08 12:07 AM (15 years, 4 months ago)

lol i wish i had read your reply before i posted that last one.  i think you essentially confirmed my theories.  wish i had gotten this conclusion before i wasted an inordinate amount of naptha.  lesson learned (hopefully).  im much obliged


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