soo ive got a bit less than 2g of spice in a beaker, i slowly added 100ml of heptane. setting it settle and pulling it off every 25ml. as i pulled it off much dmt was still solid at the bottom. the heptane instantly turned yellow! as i pulled more and more solvent thru the beaker, the solid spice kept getting WHITER AND WHITER!!! my re-x was working backwards....

this is the first time i tried to clean my spice with room temp heptane, not hot. i assumed it would pick up less yellow, but instead it is JUST picking up oils.

i took 1.2g of tan/pink/orange fishscale in a 10ml vial. to this i added about 8ml of heptane. i pulled, evapped in an AL dish over a triple boiler. i did this with about 24ml. upon evap, it yielded nearly exclusively oil that finally hardened 15min-45 later.

why cant i get my spice white guys? it just seems like every time i try to clean it up using a cleaning tek it just does nothing for me and i loose product.

using bestine for re-x and kleenstrip vmp for initial.

Heptane becomes more non polar as it heats up.

100ml is too much per 2g beaker. Evaporating and not freezing will also result in less pure product.

Read the instructions for recrystalization in FAQ and tell us how it went. Dont throw anything away and you wont lose yield, or if you do and its an active yield, it can be recovered.

btw, AFAIK naphtha gets more POLAR as it warms up (this dissolving slightly more polar impurities/alkaloids as the heat goes up)

tangarine,

As long as you have not thrown anything away you are fine. Just take your yellow oil and anything else you have left over from the extraction, and redissolve in a shot glass with about 25-30 ml of hot heptane. Mix around for a second, then wait for the yellow stuff to stick to the bottom of the glass. Pull the heptane up with a glass eyedropper, it should most likely get cloudy in the dropper, then put it into your collection jar/tray and freeze precip. You should recover the majority of your pure white.

endlessness,

At what temp does naptha become polar, or more polar? I always used to use HOT naptha, but would always freeze precip after. I never noticed any impurities on the first 5 pulls, but when reheating the bark mixture, adding hot naptha, mixing, and then pulling, the end result would always be yellow crystals. I now only use heptane throughout the entire extraction.

does this mean youve replaced naptha w/ heptane?

Yea, Im pretty sure naptha consists of heptane and other nonpolar solvents. Almost as though naptha is a less pure heptane.

jimm,

Yes, naptha has been replaced with heptane throughout the whole pulling and recrystallize process. Heptane is pretty expensive though.

True, but it can be reused many times. Also, I much prefer the rubber cement smell of heptane to the dirty gasoline smell of naptha. Some may disagree though.

-JM

True, but it can be reused many times. Also, I much prefer the rubber cement smell of heptane to the dirty gasoline smell of naptha. Some may disagree though.

-JM[/quote]

Problem SWIM has with heptane is he always likes to evap most of the solvent before freeze precip, so he loses the majority of the solvent.
For some strange reason, I dig the smell of naptha, heptane is definitely a lighter smell though

Interesting. I never thought evaporation was necessary with heptane because it's so bad at holding onto spice at freezing temps. Does SWIY find that they get a better yield after evaporating or is there some other reason?

Well, SWIM never did either. But one day he did two separate 50 gram batches using his hybrid tek and did his pulls with heptane like normal. On one he collected his four pulls into his tray and put directly into freezer. On the other he collected the four pulls, but instead put in front of a fan for about 6-12 minutes (does not take long to reduce to desired amount)and then put into freezer. SWIM will notice the evaped solution get VERY cloudy before putting it in for the precip. The evaporated pulls precipitated out faster, and yes, SWIM noticed better yields, maybe about an extra 100 mg or so of spice, but SWIM can't remember exactly anymore since he always evaporates first now.

That's good info, thanks. I've seen used heptane evaporated completely to produce oils that were assumed to be n-oxides or plant oils mixed with N,N-DMT. Quite active, but not fluffy crystals like with a freeze-precip. So it serves to reason that there is some spice left in the solvent, even after long freeze precips of 48-72 hours. Not sure of temp in the freeze area though. That could definitely be a factor.

How long does SWIM freeze precip? Any idea of temp?

I wonder if reusing the heptane for more pulls reduces any losses over time, since any spice still in solution after a good freeze precip will just stay there. Like a threshold amount from the first pull that may never come out via freeze-precip, but on successive pulls there's no additional loss. So the amount of heptane used could be minimized by reusing it a few times, then eventually evaporating it to get the last bits out.

Anyway, reusing the heptane over and over again seems to work pretty well from what I've seen and yields are close enough to those from extractions on the same bark using fresh solvent that I think it makes sense economically, health-wise and environmentally. 100mg spice is only about 10g bark, after all. That's about $2-$2.50 according to my calculations using relatively high prices. In other words, a loss of 100mg @ $2.50 costs relatively little compared to the $9 (~500ml heptane @ $15, a pretty high price) it would cost to do 3x100ml pulls and evaporate the heptane away without reusing it.

Thanks for discussing this- I'm always interested in comparisons of techniques and materials. Please don't take my comments as a critique of your approach, just a quick and dirty comparison to explore the differences. YMMV, of course, and your personal preference is something I have to respect.

-JM

One thing I neglected to mention in favor of the naptha approach is that it's much cheaper, as stated previously in this thread. A quick comparison shows that Bestine heptane is about 3x more expensive than generic VM&P naptha. Certainly a factor if solvent re-use is not employed. Heptane is still preferred in these parts due to the 'more tolerable' smell and a perceived cleaner end product, though.

-JM

Im with you on the heptane is more pleasant to work with over naptha bit, I do the orangeness too tho, on occasion...

SWIM is lucky enough to have a store around that sells Bestine for $11, while VM&P naptha is $7. The only thing is that the Heptane is a 16oz container, while the naptha is a full quart. So the price difference is actually closer to what you said jmaxton, when you compare exact volumes. In the end though, SWIM gladly pays the extra money for a smaller bottle of heptane because the results are so much better. Some things in life just cost more...

Jimm- Are you saying that the orange 'impurities' (for lack of a better word) allow for more consistent breakthroughs? That's very interesting. Mind if I ask about the vaporizing method used? I've definitely noticed a difference between the pure white and the yellow goo, but neither seems to work better in terms of entering hyperspace and breaking through. Just different experiences when the destination is reached. The experience with the yellow seems more liquid and bubbly while the white seems more sharp and detailed. Maybe that's all placebo, as the yellow goo is actually more liquidy and the white crystals are more sharp. I'm referring to the physical characteristics of the substances in that last sentence, just to be clear. I wonder if a double-blind test would show the same results and if others' experiences are similar.

I've heard several Nexians say that the 'jungle' produces a more smooth and less jumpy/erratic experience than the fluff, but I don't have any first-hand knowledge with jungle- just yellow oil, earwax and white fluff. Is this orange you speak of akin to the jungle or something different, perhaps a middle ground between white crystals and jungle? Otr is it the same as the earwax I sometimes see?

I thought jungle was normally pulled with xylene or limo but I absolutely hate the smell of xylene and limo requires salting and then free basing, which increases losses significantly in the experiments I've seen.

I'm interested to hear others' takes on this. Thanks!

Agreed!!! Heptane rocks!

jmaxton- Im new to this and been playing around for about 2 months now, need to get a "machine" or a GVG.

my friend seems to always get to a nice place w/ the orange, hit or miss with the white.

Oh yeah, the machine is where it's at. Very easy to use, and VERY effective for SWIM and his friends.

Bestine to Naptha 1:1 according to Norman's Tek?