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failed process, damage control please... Options
 
mew
#1 Posted : 7/27/2012 1:36:09 AM

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after salting dlimo with vinegar
evaporating the vinegar
and converting with washing soda
pulling with dry ipa
the freebase is still a dark orange goo, it smells of spice an not of ipa or vinegar

i think its contaminated with dlimo
should i add more water and siphon of dlimo (wont the freebase be soluble in both dlimo and water though? id lose some product, unless i resalted from the dlio i isolated)

or freeze it and see if i can pour off some dlimo, in which case id try resalting it anyway to see if there was a yield loss


thank you~
 

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MelCat
#2 Posted : 7/27/2012 1:43:56 AM

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I don't have much experience with d-limo so I can't really chime in there.

My first thought, if you don't have any beef with petro chems, is to re-x the goo with some heptane.

You won't lose any product this way and you'll end up with some amber crystals when the orange goo dries and some lovely yellow/orange crystals from the pure spice that's in there. You can get closer to white with further re-x's if you choose.
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The Day Tripper
#3 Posted : 7/27/2012 1:47:52 AM

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Have any fumaric acid?

If you did fasi, it should remove any traces of dlimo as it would be soluble in the ipa. Then just base it again, and pull with ipa to get freebase w/out any limo.

You don't even have to do fasi either, you could just dissolve the freebase in fasw, evap and wash 2x with dry iso or tone, then base and pull.

Either way would remove any traces of limo.
"let those who have talked to the elves, find each other and band together" -TMK

In a society in which nearly everybody is dominated by somebody else's mind or by a disembodied mind, it becomes increasingly difficult to learn the truth about the activities of governments and corporations, about the quality or value of products, or about the health of one's own place and economy.
In such a society, also, our private economies will depend less upon the private ownership of real, usable property, and more upon property that is institutional and abstract, beyond individual control, such as money, insurance policies, certificates of deposit, stocks, etc. And as our private economies become more abstract, the mutual, free helps and pleasures of family and community life will be supplanted by a kind of displaced citizenship and by commerce with impersonal and self-interested suppliers...
The great enemy of freedom is the alignment of political power with wealth. This alignment destroys the commonwealth - that is, the natural wealth of localities and the local economies of household, neighborhood, and community - and so destroys democracy, of which the commonwealth is the foundation and practical means.” - Wendell Berry
 
mew
#4 Posted : 7/27/2012 1:47:55 AM

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yea, no interest in petro chems

freezing for the last 20 min made a whitish cloud in the thin layer of goo
 
mew
#5 Posted : 7/27/2012 1:49:51 AM

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whats heptane got that dry ipa aint got?
 
mew
#6 Posted : 7/27/2012 1:50:35 AM

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yes i do have fasi/fasw

 
mew
#7 Posted : 7/27/2012 1:52:50 AM

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dosent fumaric tend to create yield loss by not salting the oxide of dmt

even if that were the case, i could just keep the dlimo contam with n, n oxide for separate use
 
MelCat
#8 Posted : 7/27/2012 2:09:18 AM

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mew wrote:
whats heptane got that dry ipa aint got?


It's just a better solvent for forming the beautiful crystal clusters.

Most of the freebase spice pics in the just some xtals thread were re-x'd with heptane aka Bestine. It does a wonderful job at creating crystal porn if allowed to cool/evap slow enough.

Edit: This is a full spectrum crystal re-x'd with heptane.
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The Day Tripper
#9 Posted : 7/27/2012 2:11:57 AM

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mew wrote:
dosent fumaric tend to create yield loss by not salting the oxide of dmt

even if that were the case, i could just keep the dlimo contam with n, n oxide for separate use


If you fasi it, then yes. I notice the oxide is somewhat soluble in the ipa. But if you fasw it, and wash with just a few mls of ipa 2x it should not be significant.
"let those who have talked to the elves, find each other and band together" -TMK

In a society in which nearly everybody is dominated by somebody else's mind or by a disembodied mind, it becomes increasingly difficult to learn the truth about the activities of governments and corporations, about the quality or value of products, or about the health of one's own place and economy.
In such a society, also, our private economies will depend less upon the private ownership of real, usable property, and more upon property that is institutional and abstract, beyond individual control, such as money, insurance policies, certificates of deposit, stocks, etc. And as our private economies become more abstract, the mutual, free helps and pleasures of family and community life will be supplanted by a kind of displaced citizenship and by commerce with impersonal and self-interested suppliers...
The great enemy of freedom is the alignment of political power with wealth. This alignment destroys the commonwealth - that is, the natural wealth of localities and the local economies of household, neighborhood, and community - and so destroys democracy, of which the commonwealth is the foundation and practical means.” - Wendell Berry
 
mew
#10 Posted : 7/27/2012 2:35:11 AM

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@ day tripper

lets say theres 1 oz of freebase semi viscous liquid. what would you do from here?
 
The Day Tripper
#11 Posted : 7/27/2012 3:18:52 AM

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Wow 1oz of freebase!!

Well, add 30% by weight of fumaric acid to hot distilled water until its all dissolved, and add the freebase. If it all doesn't dissolve add a little bit more fumaric acid to see if it helps dissolve. But 30% is liberal as far as fumaric acid, its more like 22-25% to salt the dmt. Since your basing it later it doesn't really matter to use a bit excess to be safe. Then filter it if theres particulate, and evap.

It prob won't harden up until you scrape it up and work it around, but if you wait a few days it will crystallize w/o scraping. I usually just scrape the goo and work it until it becomes milky colored and thicker, finally hardening up. You can dry it in ~15min this way vs a few days for just letting it sit.

Then wash that with minimal ipa. There shouldn't be much dlimo in it since the fasw would not be soluble w/ it, so minimal ipa washes should be more than enough to get the last bit of limo. If you have acetone, use it instead as the fumarates are much less soluble in it.

Then base w/ caoh or sodium carb paste method, dry and pull with ipa for full spectrum freebase. You could pull w/ heptane a few times if you want to get the n,n freebase, and then ipa or acetone to recover the oxide/other alkaloids if you want them separate. Not sure how to seperate them w/o petrochems though.
"let those who have talked to the elves, find each other and band together" -TMK

In a society in which nearly everybody is dominated by somebody else's mind or by a disembodied mind, it becomes increasingly difficult to learn the truth about the activities of governments and corporations, about the quality or value of products, or about the health of one's own place and economy.
In such a society, also, our private economies will depend less upon the private ownership of real, usable property, and more upon property that is institutional and abstract, beyond individual control, such as money, insurance policies, certificates of deposit, stocks, etc. And as our private economies become more abstract, the mutual, free helps and pleasures of family and community life will be supplanted by a kind of displaced citizenship and by commerce with impersonal and self-interested suppliers...
The great enemy of freedom is the alignment of political power with wealth. This alignment destroys the commonwealth - that is, the natural wealth of localities and the local economies of household, neighborhood, and community - and so destroys democracy, of which the commonwealth is the foundation and practical means.” - Wendell Berry
 
Dr_Sister
#12 Posted : 7/27/2012 3:56:59 AM

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mew wrote:
whats heptane got that dry ipa aint got?


Heptane is a very non-polar solvent, IPA is a polar solvent. Heptane, Hexane or Naptha are all very selective. Meaning they will get the dmt, but leave most of the other contaminants behind. If you did you initial pulls with one of these non-polar solvents you would not be having these problems with orange goo, or it would be much less an issue.

The downside is that they are so selective they usually take larger quantities of solvent to extract the same amount of spice. But, IMHO they are the only way to go.
 
mew
#13 Posted : 7/27/2012 4:44:27 AM

huachumancer


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thank you for the support!

@ daytripper, i meant to say 1 liquid oz, lol!

@dr sister, i avoid petrochems for personal and legal reasons, its much more feasible that one have orange oil and ipa than it would be more traditional solvents. mew just like being safe, even if it means going that extra mile

on another note, if i wanted to keep some as fumarates how would i clean up the excess fumaric acid? going to check the wiki i might answer my own question Smile
 
mew
#14 Posted : 7/27/2012 5:21:03 AM

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i weighed the goo, and its 28 gs... so yea 1 oz in 20 mls
 
mew
#15 Posted : 7/27/2012 8:55:20 AM

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so heres whats up since my goo weigh...

i added 9 g fumaric acid to aprox 150 ml distilled water. i mixed this into the freebase goo, shook vigoriously for 10 min, put in hot bath, shook vigorously until i totally dissolved the fumaric acid.

let it sit hoping some dlimo would rise and i could separate it from the fumarate liquid, it didnt, so i proceeded to evaporate the fumarates slightly discouraged. using a hotplate and only steaming the fumarates, it eventually started to bubble, around the bubbles were dark clouds forming, i stirred and teh entire solution took on a darker color, thinking that this was the end of the water in my fumarates i let it go for a minute, it started to smell really funny and the steam turned into smoke.

i took it off and manually crystalized a hardish ball, that still had a sticky consistancy, realizing i had started to vaporize the dlimo and thats what had burned, but my fumarates were dryer than my acetates had been.

i looked up the bp of dlimo 176 °C, and the bp of fumaric acid is 287 °C, perhaps i could vaporize the dlimo to ultimately make my fb a non goo. so i put it back on and let it burn off, smoke piped off and i took it off prematurely as i was worried by the amount of smoke it produced (in my house), it dried ROCK HARD, no goo at all,

i tried scraping it but it just shattered into shards and were impossible to keep in the dish, i just put water on it and began trying to mix it in, chunks of brownish black sticky stuff collected and floated at the top, assuming it was the non polar remnants of the dlimo vaporization i just went ahead and tried mixing it in anyway, it didnt work. i added washing soda and the chunks stayed sticky and non dissolving, the water turned a rusty orange color and neutralized the fumarates. i decided to add a bit of ipa to it to dissolve the sticky chunks, it worked! they all dissolved and there seemed to be more reaction taking place. i theorize that the non polar chunks encapsulated some fumarates but only realeased them when i dissolved them with ipa.

i stirred it through thoroughly and dissolved all the chunks leaving me with a dark dark ipa on top of whitish orange washing soda. using a hair dryer on "cold" i evaporated some and stirred, more reactions took place. i assume that the lack of ipa to suspend the newly released fumarates forced the fumarates into contact with the base, nuetralizing them. ( i did the ipa part 2 hours into the fruitless stirring of the nps chunks ) i reduced again and again stirring the darkening ipa back into the base and observing more neutralization.

im leaving it for the night to totally dry out and will add a bit of water once the ipa dries to ensure that everything has been freebased. when that water is evaporated, ill chop it up and put it in a jar, add dry ipa and shake, let settle decant off ipa, repeat till ipa is clear, then place sediment into filter and wash with ipa to get all the remains.

when the collected ipa is dry ill add a bit of water and hopefully separate the freebase (which will dissolve) from the non polar burn residue (which should float) running this through a filter and washing with a bit of water. ill keep the water and evaporate it with a fan to hopefully yield clean dry freebase!!!!
 
Infundibulum
#16 Posted : 7/27/2012 4:57:22 PM

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Why do you suspect limonene contamination in the first place? your OP does not even idicate something line that. I think you're trying to solve a problem you do not have.


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

 
benzyme
#17 Posted : 7/27/2012 5:07:48 PM

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Dr_Sister wrote:
The downside is that they are so selective


I've seen the term 'selective' thrown about recently. AFAIK, no single solvent system is selective, that is, heptane will not exclusively pull dmt (this is why solvent partitioning and/or chromatography exist). dmt has poor solubility in heptane, because of the lack of pi-bond conjugation, which is why it's a better recrystallization solvent.
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jamie
#18 Posted : 7/27/2012 5:13:26 PM

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I dont think there is limo contam..I think it is from the vinegar..that and you prob have oxides in there that make it oily..
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mew
#19 Posted : 7/27/2012 7:26:59 PM

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at this point, the freebased fumaric+washing soda mixture is nearly dry, ill give it a few more hours then pull till exhuastion with dry ipa, evap and judge the new product
 
mew
#20 Posted : 7/28/2012 6:34:29 AM

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theres roughly 700 ml of dark dry ipa. 10 ccs were evaporated and it yielded burn orangish tar and whitish liquid, the tar seems to carry a faint tryptamine odor, and the liquid i assume is water, meaning my dry ipa/washing soda conversion wasnt entirely anhydrous.

comparatively to 10 ccs of the original freebase goo which smells of dmt the new "freebase" dosent smell a lot like it, infact upon vaping some to get an odor, there seems to have been no tryptamine smell. wtf?!





ok so this is now a damage control situation, or did i totally ruin this batch by trying to vape off the suspected limo contams on a hot plate while the dmt was fumarates? ughhh!
 
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