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Next logical step in Acetone drytek with Sodium Carbonate?? Help, in middle of extraction. Options
 
crakkbakk
#1 Posted : 6/17/2009 11:25:33 AM
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I mixed 50g of MHRB and 50g sodium carbonate with some water to base in a "drytek" manner and extract with acetone and evaporated.

What next? Evaporate yielded a tan powder.
 

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Phlux-
#2 Posted : 6/17/2009 11:43:15 AM

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well if there was any water what so ever still on the drytek gunk it would have mixed with the acetone - so ur evap could contain plenty sodium carbonate and other random stuff from the bark.

perhaps best thing to do from there would be convert the tan powder to a fumarate or other salt form - clean then re-freebase it.
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crakkbakk
#3 Posted : 6/17/2009 11:59:22 PM
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There was no water visible.

I do not have fumaric acid availible.

I'm thinking of trying a recrystalization or even an A/b...

Any more ideas?
 
Infundibulum
#4 Posted : 6/18/2009 12:29:37 AM

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(Re)crystallisation of the resulting powder using naphtha is a good idea. Your end-result powder should contain the freebased spices, plus lipids plus other stuff. Mixing the warm naphtha with the powder and then freeze-precipitating wil give a much cleaner product.

You can also try to smoke some of the tan powder just to verify that something of interest to-be-recrystallised is indeed present! Something like 20-40mg will definitely tell you if spices are present.

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crakkbakk
#5 Posted : 6/18/2009 11:10:59 AM
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The tan powder was scraped and added to hot napthta, filtered (some black junk in filter), allowed to cool to room temperature, placed in recrirgerator for a length of time and finally placed in freezer. In the morning it will be collected and observements will be made.

It is possible that I used too much naphtha for it to precipitate. If this is the case, I will filter it, evaporate it down and try again.

Question: in this circumstance, was a recrystalization with hot napthta to a slow cool beneficial? It seems to me that hot napthta pulls more inactives, and when it cools more inactives will crash out with the spice. Would room temperature napthta have been better?
 
Phlux-
#6 Posted : 6/18/2009 11:13:17 AM

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hot naphta is fine - the spice should precip if the naptha was evapped down a bit - it should turn milky when u blow on it - then u know its ready for freeze precip.
antrocles wrote:
...purity of intent....purity of execution....purity of experience...

...unlike the "blind leading the blind". we are more akin to a group of blind-from-birth people who have all simultaneously been given the gift of sight but have no words or mental processing capabilites to work with this new "gift".

IT IS ONLY TO THE EXTENT THAT WE ARE WILLING TO EXPOSE OURSELVES OVER AND OVER AGAIN TO ANNIHILATION THAT WE DISCOVER THAT PART OF OURSELVES THAT IS INDESTRUCTIBLE.


Quote:
‹Jorkest› the wall is impenetrable as far as i can tell


Quote:
‹xtechre› cheese is great


He who packs ur capsules - controls your destiny.

 
endlessness
#7 Posted : 6/18/2009 11:45:32 AM

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Yes warm naphtha pulls more inactives, but on the other hand, if not enough room temperature naphtha is used (or when it cools), then maybe some dmt will crash out together with the actives...

SWIM always makes 25ml warm naphtha per g of impure dmt, seems to work fine for him.

BTW, SWIM has noticed that cloudiness by itself is not a good indicator of saturation of naphtha.. It seems for some reason, specially when fast-evapping in front of a fan, that the naphtha gets cloudy quite soon after one leaves it to evap.. Then, after a while, it becomes transparent again, and only later it becomes cloudy and fully saturated. At least this happened to SWIM a few times. and since there is no problem of overdoing the 'pre-evap', SWIM would recommend leaving only small amounts of naphtha when putting in the freezer.

As for the cooling down slowly, the only advantage AFAIK, is to grow larger crystals (specially if one keeps alternating between freezer/fridge a few times before leaving in the freezer for long in the end), but purity wont be affected, I think, because whatever impurity is there, will be there anyways.
 
crakkbakk
#8 Posted : 6/18/2009 9:37:56 PM
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Today Swim looked in the dish in the freezer and saw a lot of white in there which made him excited, but after he filtered the napththa off and scraped it he realized that most of the white was just frost and there was some brown shit. He put the solids in a piece of filter paper and squeezed it, after drying he saw only a couple beads of black.

I decided to throw that shit out. I think that I didn't make the dish air tight enough which let frost get in. Does this make sense?

I'm going to evaporate the naptha down a bit and then evaporate, I did use too much naphtha.

Right now the naphtha is a piss yellow color like I normally get from STBs with water and NaOH.


With the jar of the gunk I added naphtha too it (originally I used acetone, evaporated it and then attempted a recrystalization with naphtha) and I'm going to see what I get later tonight.



On a side note, is any of the DMT in MHRB in its natural state soluble in naphtha/acetone (before the base is added?) If so one could wash with either acetone/napttha before basing?
 
crakkbakk
#9 Posted : 6/19/2009 9:45:21 AM
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Swim evaporated the "acetone pulled" naphtha down to a very tiny amount and placed it in the freezer. It shouldn't be a problem if the amount of naphtha was very small, should it?

Swim mixed naphtha earlier in the day with the basifyed MHRB, filtered it and had a very clean, slightly yellow (very slight) naphtha that had a good bit of an oil that wouldn't disolve in the naphtha...couldn't have been water as none was used, might be dmt-oxide? The MHRB is relatively old.

Swim put the new non-acetone naphtha in the freezer as well.

Will report in the morning.
 
crakkbakk
#10 Posted : 6/19/2009 7:59:20 PM
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Fuck!

Both naphtha were evaporated. The acetone'd pulled-naphtha evaporate yielded nothing.

The plain naphtha yielded a good bit of yellow but upon scraping the material was infused into my filter paper.

Fuck.

Did I use enough sodium carbonate? Should I use lye instead?

Do dryteks even work?
 
crakkbakk
#11 Posted : 6/19/2009 9:42:55 PM
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I first decided to add more sodium carbonate in case I didn't base it enough. I then decided that I was just going to add water to eliminate that variable. I'm now doing a standard STB with sodium carbonate and naphtha. If this doesn't work I will know that it is the sodium carbonate not doing a good enough job, and I will restart over with NaOH dry tek.
 
amor_fati
#12 Posted : 6/19/2009 11:48:27 PM

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Drytek with MHRB is reportedly a very touchy technique. SWIM's FOAF has gotten it to work but has neglected reporting it on here. SWIM, however, didn't have much luck with it, but was using a very small amount and very sloppy technique Embarrased . When SWIM manages to get a larger amount of MHRB, he will do more thorough experimentation. Until then, SWIM wouldn't recommend it unless one's willing to take some time and carefully test every aspect of the process to isolate the variables. SWIM hypothesizes that the consistency of the bark demands that it requires more time to basify. SWIM would recommend using a saturated solution of sodium carbonate to wet the bark and make the paste, rather than a dry premix.
 
crakkbakk
#13 Posted : 6/20/2009 9:43:09 PM
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I'll have to try that.

So I dumped it all out in a large glass bowl to let the naphtha have more surface area while I stirred.

I immediately noticed that most of the rootbark wasn't disolved in the amount of water I added, and I remembered reading in the nexus that more water always made the naphtha pick up more dmt (ironically the drytek uses no water! Maybe water is needed? More experimenting!) so I added enough water and some extra naphtha to make it fluidy.

I stirred it for 10 minutes and funneled it back into it's jar where I shook it violently for 5. I will evaporate at night time.


Something noteworthy: I have been using plain naphtha instead of vm&p naphtha. I asked on this board and people said it didn't matter. I am now doing a regular stb on 100g mhrb with naoh and the same naphtha. I am going to freeze precip it tonight to eliminate that variable.
 
crakkbakk
#14 Posted : 6/21/2009 10:28:09 AM
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the acetone=carbonate=naphtha one evaporated to a tiny 1/2 inch diamiter yellow puddle. Hopfully dmt.
 
 
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