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Fumarate to freebase loss of yeild solution. Options
 
Phlux-
#1 Posted : 8/22/2009 4:28:05 PM

The Root

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Okay so swim was doing a chali extraction and "realized something" that could be fairly important that also relates to mhrb.

Now a lot of ppl have complained about getting low yeilds when converting from fumarate to freebase and others have had no issues and i think the reason is simple - i may be wrong on this tho.

To do the chali extraction swim did an a/b then pulled with xylene and added fasa for the fumarates to precip.
first difference noted - the fumarates were like sand and not like needles at all.

The fumarates were washed - no noticible loss - so not much fumaric acid contamination - a lid was used while the fumarates formed to prevent evaproation of acetone which swim thought may lead to fumaric acid precipping and the xtal formation was not disturbed.

To freebase swim made a paste with sodium carbonate and pulled with acetone when dry - huge loss noticed.

Then swim thought back to his dmt-n-oxide experiement - he had some remaining on a plate (created using hydrogen peroxide)
Swim tried disolving it in acetone - didnt work - then water - disolved fast so swim realized that the n-oxide is water soluble.

When freebasing using this method the sodium carbonate is water soluble so u cant separate the freebase using that - a base that is a gas is called for.

perhaps ammonia ?

Now how this effects the fumarate to freebase problem and variety of % lost could simply be due to the amount of n-oxide present in the bark - if that fumarate was either freebased using a gas base - yealds would be larger but n-oxide would be in the final product - fine for mixed alky extractions - or it could be converted back to nn-dmt then freebased.

Sounded like a fairly reasonable explanation to me.



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Phlux-
#2 Posted : 8/22/2009 5:12:35 PM

The Root

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this is besides the loss of weight due to having the fumarate attached.
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.

 
soulfood
#3 Posted : 8/22/2009 7:33:33 PM

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I figured the whole thing with N-oxide a while back, especially as I exaust my mix with a standard solvent first before pulling with xylene for FASA. My conversation rate on this N-oxide heavy spice is about 20%... that's to DMT, then I assumed the rest has been mainly N-oxide.

It's not really bothered me much before as I have been leaving my DMT fumerate as is for pharmahuasca, but recently I've started trying to get everything to a base and I've been realising these losses and they are definately not just from excess fumaric acid as I have been purifying x2 with water and yielding some damn nice crystals.

Rather than having to use ammonia as a base, wouldn't it be much easier to remove the DMT with standard naphtha and then pull the N-oxide with limonene and evap? I'm fairly sure N-oxide is soluble in d-limonene... then again I thought it was soluble in acetone...

What about using some good old zinc to get those n-oxides deoxidised?
 
Phlux-
#4 Posted : 8/22/2009 7:36:44 PM

The Root

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swims never managed to evap dlimonene cleanly - always a residue and swim added xylene to the acetone when it was on the n-oxide during that test he did - it didnt make any difference.
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.

 
soulfood
#5 Posted : 8/23/2009 8:54:32 PM

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hmm... stronger base maybe?
 
Jorkest
#6 Posted : 8/23/2009 10:45:07 PM

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this is an interesting topic...ill think about it abit..
it's a sound
 
Heretic
#7 Posted : 12/19/2009 10:01:22 AM

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you didn't basify high enough with the carbonate I think
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