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Fumarate after xylol help cleaning.. Options
 
Hupecat
#1 Posted : 11/28/2012 7:38:15 PM
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i knwo, hrere is a nice detaileed Sticky right above me… but it semms mine looke completeley different..?
I did some naphta pulls, and when done switched to Xylol..
i used the FASA Method, syphoned the xylol the next day, and sraped all together and let it dry…
so this is my actual product, can anybody tell me which Step, wash, solvent is next?


 

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Mindlusion
#2 Posted : 11/28/2012 9:15:47 PM

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Those fumarates look great!

Your next step is to recrystallize, your also going to want to remove the excess fumaric acid.

Hint: DMT fumarate is extremely soluble in water, fumaric acid is not so
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Hupecat
#3 Posted : 11/29/2012 8:00:24 PM
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so thx for the answer…
but does that mean just washing with water??
and who to chrystallize then?
dissolve it in naphta and do a r-ex``

will the fumarate i have look like the clean needles after washing with water???
 
Hupecat
#4 Posted : 11/29/2012 8:06:08 PM
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i read again through the sticky, but he is doing a FASA at the end of his process, wgich i already did right from beginning..
if i would add more fumaric acid now, excess like he wrote, i would have even more of the fumaric..
i think i need to get rid of it, somehow..???
 
Mindlusion
#5 Posted : 12/1/2012 8:30:57 PM

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dissolve them in very small amount hot water, and let them crystallize out over a week or so, then you will have quite pure, nice looking fumarates.

Actually, there probably isnt a whole lot of excess fumararic acid, but its easily possible for it to precipiate when added to the xylene. doing FASA again would remove any.

---

Instead of dissolving them in water, a faster method would be convert them to freebase, re-dissolve in dry acetone, and do FASA again. Youll get nice needles.. look at endlessness's thread https://www.dmt-nexus.me...aspx?g=posts&t=28417
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Hupecat
#6 Posted : 12/3/2012 2:15:41 PM
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Mindlusion wrote:
dissolve them in very small amount hot water, and let them crystallize out over a week or so, then you will have quite pure, nice looking fumarates.

Actually, there probably isnt a whole lot of excess fumararic acid, but its easily possible for it to precipiate when added to the xylene. doing FASA again would remove any.

---

Instead of dissolving them in water, a faster method would be convert them to freebase, re-dissolve in dry acetone, and do FASA again. Youll get nice needles.. look at endlessness's thread https://www.dmt-nexus.me...aspx?g=posts&t=28417


in all these teks theres something written about mixing with Sodium cabonate..
You say i shall just add water and let it chrystallize over a week?

Why should i add it to Xylene again, doing a fasa, which took me to these dirty fumarate?.
wouldn't i end at the same product again..
i thought i need to get the chrystal needles to be fumarate.free of any fumaric.?
so, no need for me to add sodium carbonate??
i'm really clueless to fumarate yet..

you suggest just a warm water wash as stated in this link??
https://wiki.dmt-nexus.m...on_of_Final_Purification

if i would go the way of endlessness, i would create some Freebase from dirty fumarates, and i dont know how i should end with clean freebase, when starting with dirty fumarate without being washed before ..
and what about the Sodium carbonate… I'm some kind of stuck here

Endlessness "Cake was created by a FASI,

my product looks more like the one in this link Type 3:
https://wiki.dmt-nexus.m...e_crystallization_method

any help still appreciated, cause i have a great batch of those dirty fumarates..

wouldnt this be the best solution for me going the way with boiling IPA??
https://www.dmt-nexus.me...&m=314263#post314263
 
Mindlusion
#7 Posted : 12/3/2012 4:53:26 PM

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Either way will work hupecat.

Sodium carbonate converts fumarate BACK to freebase.


Id stick with the water re crystallization if I were you.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Hupecat
#8 Posted : 12/13/2012 8:04:00 PM
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hey.. i followed your suggestion doing the Water-Chrystallization and this is what i got after drying..

brown reddish goo??

http://imageshack.us/pho...-images/18/fumarate.jpg/



Mindlusion wrote:
Either way will work hupecat.

Sodium carbonate converts fumarate BACK to freebase.


Id stick with the water re crystallization if I were you.

 
Hupecat
#9 Posted : 12/13/2012 8:04:45 PM
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hey.. i followed your suggestion doing the Water-Chrystallization and this is what i got after drying..

brown reddish goo??

http://imageshack.us/pho...-images/18/fumarate.jpg/



Mindlusion wrote:
Either way will work hupecat.

Sodium carbonate converts fumarate BACK to freebase.


Id stick with the water re crystallization if I were you.

 
Mindlusion
#10 Posted : 12/14/2012 12:42:06 AM

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Looks like you removed the excess fumaric acid from your fumarates.
You said you evaporated it?

its progress

Can you detail me further on what you did exactly?
Was there material that did not dissolve fully when you added water? (if so, this means this is fumaric acid, which should not dissolve, leave it behind)

What I should have mentioned its possible to collect two (grades), where after some crystallization has already begun, you pour off the solution into another container for it. One will contain mostly gunk, the other more pure fumarates.

Your still good, on the right track. You just left some of the gunk in.

--

If you want to purify further, I recommend crystallizing fumarates with boiling IPA

(Heat up IPA till boiling, dissolve the fumarates, let it return to room temperature slowly. Pour off the IPA from gunky impurities, and stick it in the fridge. Collect crystals)


Sorry for sticking you with the water method, its slow, but I misinterpreted the purity of your orginal crystals. Water re-x is great for producing, large, pretty fumarates, of fumarates that are already cleaned.

Try the IPA method
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Hupecat
#11 Posted : 12/15/2012 3:04:46 AM
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i was using the Water washing Tek

https://wiki.dmt-nexus.m...on_of_Final_Purification

word by word..

had a glas, filled in the fumarates..
then 12 ml warm distilled water per gramm as described...
The aqueous turned yellow, like healthy urin...
then filled it in some test tubes, i think i needed 3 or 4 of them, and let them settle for quite a while..
Some "dirt" was falling on the bottom of the test tubes, which i left in and decanted into this Glasdish only the yellow aqueous seeing on photo, leavin a bit of stuff which fell on the ground of the test tubes,

you can see here what was left from the aqueuous:



and left it untouched in a dark cupboard.... took quite a while....

Then i had the glass 1/5 full of some hard goey filling..,
thought i start to scrape it a bit, to let more air come in the middle to evap better...

Thats what you can see on the photo..
a gooy very adhesive reddish looking substance..??

so, and here i am now??

please help..
 
Hupecat
#12 Posted : 12/15/2012 3:13:31 AM
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Mindlusion wrote:


Try the IPA method


just read through IPA-Version,
As i have this redish goo now, would that dissole like as it should, because he starts with a yellow powder like i had in the beginning...
it was 3.5 gr of Fumarate powder when i started...

The thing i m wondering is why this has changed to this dark reddish color just by adding water??

would my goo turn n into a glass full of yellow urin looking liquid again like in the TEK..?
https://www.dmt-nexus.me...&m=314263#post314263


 
Infundibulum
#13 Posted : 12/15/2012 1:55:53 PM

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hupecat, you need to tell us what do you want the final product to be. do you want fumarates? do you want freebase?

mindilusion might have been giving you bogus advice because you are not clear as to what you want.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Hupecat
#14 Posted : 12/16/2012 7:37:57 AM
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i wanna go on Fumarates..
 
Hupecat
#15 Posted : 12/16/2012 11:04:10 AM
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Hupecat wrote:
i wanna go on Fumarates..


Short update,, as looking all good when gunk was disolved and decanted cats yellow urin
was filled in glass container where the crystals shuld be better scrapeable when dried.....
did leave it in frezzer for ca. 26 hours at minus 40 °Celsius..
she did only 1 gr for testing, but all she got is a cleaner but still reddish oily like substance,, no chrystals formed....

did another FASA tek on Xylene pulls directly .. and used 50 gr of bark, and it loos she has a howl bowl of needles inthere,, still drying a bit.. but loos quite a lot nice needles...
so that worked out greatly,...Thumbs up
 
 
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