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A/B extraction questions Options
 
endlessness
#1 Posted : 10/14/2008 9:06:51 PM

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SWIM wants to make a side by side AB and STB comparison, but first needs to know a couple of things about the AB

1-What is the desired pH for the acid part?

2-SWIM only has pH strips, so it would be difficult measuring once the mimosa is inside because of the colored water. Could SWIM just measure the pure water when it gets in the desired pH (like, let´s say, 4), and then throw the mimosa after? or would the mimosa change the pH too much so SWIM´s first pure-water measure would not be good enough? AFAIK the mimosa is slightly acidic so Im guessing a pH of 4 for the water-only is a good amount.. ?

3- SWIM read a couple of AB teks around.. Some mention boiling in the acid, some mention soaking in room temperature for long time.. what do you guys think is best? Would it be a good idea to make one overnight soak, + 2x 20mins boilings?

4-How much water is good in the acid step per soak/boil for, say, 250g mimosa? Is reducing after putting them all together necessary?

5-When basifying the filtered acid mimosa water, what should be SWIM´s aim (since pH strip would again not work with the coloured water): Stop adding NaOH as soon as water turns black? Or add a certain amount of NaOH in a specific ratio with the amount of water? If so, how much?


thanks a lot
 

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Entropymancer
#2 Posted : 10/15/2008 1:34:17 AM

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A lot of the particulars of acid/base extractions are just a matter of personal preference or convenience.

1.) The pH doesn't have to be very low to effectively extract the DMT; pH 4 or 5 seems to do the trick just fine. The Entheogen Review published an "extreme condition" A/B extraction (Mambo Pachano's) that calls for acidification to pH 1 (and basification to pH 14) to destroy any skatole in the bark, but I don't think that skatole is of any concern if you're freeze-precipitating

2.) The bark is likely to change the pH of the water, though I'm not sure how substantially (I think you'll find you're pH papers are still easy to interpret even though the bark will color the liquid red). Having the water (before adding bark) at pH 4 should be fine for an extraction.

3.) I don't think there's much point to an overnight soak, as far as I know it accomplishes the same thing as simmering, it's just slower due to the lower temperature. Three 60 minute simmers seems to get everything out; it may be overkill, but then it may not. I don't know that anyone has really investigated the optimal extraction times for an A/B extraction (I figure it's better to err on the side of overkill, because SWIM isn't the most diligent about breaking up his bark). Also, it's important to note that you don't want to boil it; boiling seems to have the ability to destroy (or more likely vaporize) some of the DMT. Instead, simmer it just below a boil, so a good cloud of steam is coming off, but the liquid isn't bubbling.

4.) I don't know how much is necessary; using a bit more liquid than it takes to cover the bark on each extraction seems to be good enough. Reducing the volume isn't really necessary, but it's certainly convenient for easier handling. (Especially if you've got a seperatory funnel, reducing the volume so it fits in your funnel with plenty of room for naphtha is a good idea)

5.) SWIM just adds NaOH until the liquid turns that slippery black color, then saturates it with rock salt. I know I've seen someone claim that you don't need to basify it that far (even with mimosa), but SWIM's experience was that basifying it any less leads to unpleasant emulsions. That grayish-colored sludgy phase just loves trapping naphtha. (The NaOH is added already dissolved into a small volume of liquid so you don't have to wait for it to dissolve and mix to see what color phase you've ended up with). Also, minor sidenote: you say the "filtered" acid mimosa water... I really don't think you want to literally filter it; the tiny particulate fibers clog filters up very quickly. It's much easier to clarify the liquid by just leaving it in the refridgerator overnight. All the fibers and other cloudy bits fall to the bottom and form a fairly firm cake; in the morning, just pour the liquid off (it's now a translucent burgundy color) and it's ready to basify.
 
endlessness
#3 Posted : 10/15/2008 2:09:34 AM

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excellent, thanks a lot man!

so the filtering is hard heh? U think even with a funnel and a cotton ´plug´?

but yeah this decanting idea sounds good.. U think at room temperature it doesnt settle to the bottom as good?
 
kemist
#4 Posted : 10/15/2008 6:23:21 AM

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What a coincidence. ILPT is just about to play with mimosa while using a\b with Citric acid, sodium carbonate and solv. DCM and petroleum spirt (40-60)


endlessness wrote:

1-What is the desired pH for the acid part?


Well it depends pH 4 is recomended but in one tek swim using supersaturated citric acid with mimosa to break down tannins to avoid emulsions. With DCM emulsions are issue. IPLT was thinking to extract with acid at pH 4, then bring it to pH 2 after filtration (decantation )
endlessness wrote:

2-SWIM only has pH strips, so it would be difficult measuring once the mimosa is inside because of the colored water. Could SWIM just measure the pure water when it gets in the desired pH (like, let´s say, 4), and then throw the mimosa after? or would the mimosa change the pH too much so SWIM´s first pure-water measure would not be good enough? AFAIK the mimosa is slightly acidic so Im guessing a pH of 4 for the water-only is a good amount.. ?

Just take little bit of acidic mimosa liquid dilute with distilled water(make sure pH of water is just 7 ) and then measure the pH.
endlessness wrote:

3- SWIM read a couple of AB teks around.. Some mention boiling in the acid, some mention soaking in room temperature for long time.. what do you guys think is best? Would it be a good idea to make one overnight soak, + 2x 20mins boilings?
ILPT will definitelly simmer it gently (prob. in water bath) cos acidic solution is pretty stable and mimosa is tough material. You wanna be sure that everything would be extracted in first A step.
endlessness wrote:

4-How much water is good in the acid step per soak/boil for, say, 250g mimosa? Is reducing after putting them all together necessary?

ILPT rather using more then teks saying(just to be sure everything went to acidic water)and then he gently reducing the combined extract and filtering while hot.

Hope it would help. Very happy ILPT gonna be busy but he will be back with report and yield. BTW why swim didn`t try pH meter for hydrop. an aquariums. Parrot get it on e-bay for 14 quid (inc. next day delivery)
All the best.Wink

As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
endlessness
#5 Posted : 10/15/2008 3:58:19 PM

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thanks for the answers too Smile

SWIM doesnt get a pH meter because he really has no money right now (plus he doesn´t live in USA).. but will sometime

btw, anybody knows how much of glacial acetic acid is needed to acidify, say, 1l of water to pH 4?

thanks Smile
 
Entropymancer
#6 Posted : 10/15/2008 11:15:25 PM

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endlessness wrote:

so the filtering is hard heh? U think even with a funnel and a cotton ´plug´?


A cotton plug might work, but it's just so easy to let it all settle.

Quote:
You think at room temperature it doesnt settle to the bottom as good?


It probably works about the same, but it might take longer to settle. I just recommend the fridge since DMT is so soluble in acidic solution, and there could be other slightly slouble components that fall out.

You could experiment by leaving half your batch in the fridge and the other half at room temp, see what difference it makes.
 
Infundibulum
#7 Posted : 10/16/2008 1:09:06 AM

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endlessness wrote:
btw, anybody knows how much of glacial acetic acid is needed to acidify, say, 1l of water to pH 4? thanks Smile


0.04 grams of glacial acetic acid (=100% acetic acid) per litre will give you a pH of 4 at 25 C. Note that if one is planning to boil or shimmer the acid extraction, then some of it will evaporate. Acetic acid boils at 118 C; even if one just shimmers, plenty of it will evaporate giving one's kitchen a vinegary smell. 0.1 grams/litre will give you a pH of around 3.8 and will certainly correct for any losses due to its evaporation during shimmering.

The latter amount equals to 0.01% vinegar, fairly easy to make from commercial vinegar sources.

As for pH meter, SWIM does not have one neither he's ever intending to buy one. He's going dead cheap making his own from red cabbage. It has never let him down.

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

 
endlessness
#8 Posted : 10/16/2008 1:30:12 AM

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great thanks for the info... but btw.. 0.1g of acetic acid, lol.. and SWIM bought a liter of it.. so SWIM will use what, a drop per l or smt? haha
 
Infundibulum
#9 Posted : 10/16/2008 12:04:17 PM

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1 litre glacial acetic acid is enough for one's lifetime, maybe even enough for one's grand children's lifetime as well.

As to how to measure it, just measure 0.1 g of the liquid using a scale or something, if one desires accuracy. Otherwise 5-10 drops / litre (this is my rough estimate) are going to be enough.




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

 
endlessness
#10 Posted : 10/17/2008 12:36:31 AM

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ok so SWIM began doing the A/B today, so that tomorrow the Acid and filtering (and maybe reducing) part of it is all done, and then SWIM can do the side by side STB to compare, all synchronized...

now the thing is.. SWIM is doing 300g at a time.. so SWIM first acidified 1l of water to pH 4 with glacial acetic acid, but then when putting the powdered mimosa in the water, it seemed too thick, so SWIM thought this 1l water was not enough.. so SWIM added another 800ml or so of pH 4 water.. (was SWIM right to add more water, or is 1l enough for 300g of powdered mimosa?)

here´s how it looks:



now the problem is, this is the pot SWIM will use for the base step... It fits 3,2l... So if SWIM needs to filter/decant and repeat twice more, this will yield a total of at least 5l of filtered acidified liquid.. So SWIM will have to reduce this to half the size for the base part... But many people mentioned not to boil.. so how should SWIM reduce it all, without boiling? or is boiling ok?
 
endlessness
#11 Posted : 10/17/2008 5:10:58 AM

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Edit: ok so swim found that filtering over some old t-shirt and then squeezing the last bit out is the best.. but the filtering is not so fine. Is it necessary to make some very fine filtering or just some coarse t-shirt sieving is fine? I guess coarse filtering is fine, after all, in STB all the pieces are still inside, heh?


thanks Smile
 
endlessness
#12 Posted : 10/17/2008 6:31:39 PM

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edit: SWIM already filtered it all.. now in reducing part

so again, is a final reduction by boiling ok? will much of actives be lost this way? I mean, ayahuasca people boil for hours, can it be so bad?

SWIM´s STB vs A/B comparison + jungle spice from both has started.. results come tomorrow or day after Very happy
 
kemist
#13 Posted : 10/18/2008 7:30:07 AM

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Just simmer it gently on very low heat in wide pan for quicker evaporation. This time will ILPT use small pan inside larger pan with water bath. ILPT wanna be sure there is no more then 80 C in solution. Last time he was in hurry and boiled it off straight on the gas stove and wasn1t really satisfied with result. Now he will take his time to perform better.
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
Entropymancer
#14 Posted : 10/18/2008 8:20:25 AM

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Reducing the filtered material is absolutely fine, as long as you simmer, not boil. Like you say, ayahuasca can be simmered for hours, it's not destroying/vaporizing any DMT unless you bring it up to a full boil.

After you reduce it, you may want to let it sit in the fridge overnight to let any particulates fall out, but that's not necessary by any means.
 
kemist
#15 Posted : 10/18/2008 9:56:39 AM

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Entropymancer wrote:
Reducing the filtered material is absolutely fine, as long as you simmer, not boil. Like you say, ayahuasca can be simmered for hours, it's not destroying/vaporizing any DMT unless you bring it up to a full boil.



Acidic salt of DMT wouldn`t vaporize we are here more worried about thermolysis(high temp. degradation ) . For sure water cannot boil by higher temperature then is it boiling point (100 C) unless higher pressure then atmospheric is applied. ILPT is more worried about the tiny areas where flame directly touching the metalic bottom of pot and could increase temperature much higher then 100 C in the certain tiny little area. It`s recomended to use water bath or double bottomed pot with water used for heating up the milk.
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
endlessness
#16 Posted : 10/18/2008 3:55:01 PM

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SWIM finished. man, was this a trouble.. with only few hours of the house alone, SWIM had to rush, was hectic

Jungle spice is still evaporating, results tomorrow.. Also all the naphtha from the freeze precipitations were put together in a glass and will be very slowly evaporated over the next weeks to make large crystals out of whatever was left.


Yesterday was not SWIM´s day.. loads of things went wrong, he broke his friend´s nice pipette, a lot of solvent fell down on the floor because SWIM´s freeze precipitation container (petri dish) was overfilled.. plus the yield was total crap.. 2g out of 300g A/B + 300g STB of jurema Sad SWIM is used to 1%, and the mimosa was for sure good. SWIM hopes there will be considerably more in the slow evaporation glass and in the jungle spice. SWIM made the mistake of rushing things too much, stiring the solvent and basified mix too little times and only made 3 non-polar pulls + 1 toluene pull


oh well, thats life

BTW.. Yield of AB and STB was the same, quality also exactly the same.. SWIM will never make an AB for mimosa again, way too much trouble for nothing
 
Infundibulum
#17 Posted : 10/18/2008 6:20:30 PM

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Quote:
For sure water cannot boil by higher temperature then is it boiling point (100 C) unless higher pressure then atmospheric is applied.


Of course it can. Only pure water boils at 100 C at physiological pressure. The presence of ions and other solubles increase the boiling point as well as the melting point of water. Sea water or salt water have higher boiling and lower freezing/melting temperatures that pure water. My guesstimate would be that water containing MHRB extract would boil at around 110-120 C.


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

 
kemist
#18 Posted : 10/19/2008 6:37:54 AM

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Infundibulum wrote:

Of course it can. Only pure water boils at 100 C at physiological pressure. The presence of ions and other solubles increase the boiling point as well as the melting point of water. Sea water or salt water have higher boiling and lower freezing/melting temperatures that pure water. My guesstimate would be that water containing MHRB extract would boil at around 110-120 C.



He apologise for bad interpretation. Inf., you absolutely right acidic mimosa soup would have higher boiling point Wink But He was talking about WATER not a sup,mate Laughing ILPT has no idea how high is boiling point of mhbr soup since he hasn`t thermometer on him. He need one and then he can measure temperature on inner surface of stainless steel pot filled with water (then with soup )and placed on high flame of gas stove He knows that red spectrum from fed hot plate of electric stove is 600 C and more Those are the temperatures ilpt concerned about. 100 or 120 doesn`t make much difference but 600?
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
 
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