Better to use more solvent with small extraction? (1st STB)

[jayjay001]

I started my first extraction just a few days ago (a STB with lye, powdered MHRB, and heptane(bestine)) and I made it really small as a bit of a test run. Just about 28g of RB and Lye with around 650ml of water. I wasn't sure if I should worry about having such a small amount of heptane for freeze-precipitation wouldn't work as well. I also had no clue if adding more would have any negative effects, and I'm not talking about wasting anything.

 

[geko42]

if you are planing to freeze precipitate, then you want less fluid. but swim believes it is easier to pull the solvent if you add a little more then evap it down about 25 - 50 % and freeze. but with that small bit you could just place in a glass dish and evap it all. might not be all perfect white but you can always re-x.

 

[geko42]

ps swim sugests you do a 50 gram extraction it makes it all easy.

swims first time did 50 grams mhrb 50 grams lye, 750ml h2o and 125 - 150 ml ish naphtha evaped it all down and got a great yield. (yes i know every one is gonna say to much naphtha)

 

[abusedtoaster]

Number of pulls - STB - Welcome to the DMT-Nexus

 

[jayjay001]

Oh, thanks for the link on how smaller pulls get a higher percentage of dmt pulled. I was worried that having too little of the solvent might somehow make it evaporate too quickly before crystals form but I'll just try to make the pulls as small as possible (of course there's so little here that might be a challenge).

I'll definitely be going with a slightly larger extraction next time. Trying to be precise with ratios with so little material is a pain.

 

[benzyme]

i don't know who came up with this this 1 to 1 ratio of mhrb to lye, but it is absurdly excessive. whoever made that decision probably assumed a stoichiometric ratio, but mhrb isn't 100% dmt

 

[geko42]

You are right Benzyme MHRB is not 100% dmt.
Is there an issue that arises from using excess lye?

as of right now this is the only ratio swim has tried and it works great, and lye is very inexpensive,

edit: i wish there was a tone font.
swim read this and realized it came off wrong i am actually curious if using excess lye is gonna cause problems or if its just a waste.

 

[benzyme]

no worries

the issue is excess lye exceeds the pKa of a lot of other compounds present, so the product is pretty dirty; but that's what re-x is for... however, I'm a bit skeptical of a single nonpolar phase separating other alkaloids, and despite reporting high yields, nobody does melting point tests on their product.

what re-x won't resolve is the oxidation caused by the excess OH- ions, and that's probably why people are tinkering so much with zinc and other fad teks which attemt to reduce the oxide. they wouldn't need to fool with reduction if they followed a proper pKa curve.

 

[endlessness]

What amount of oxidation are you talking about? I havent seen any evidence for significant amount of oxidation and if it's just small amounts of n-oxide, it seems equally psychoactive and I wouldnt say it unwanted.

DMT extracted with any common tek when correctly followed will yield quite pure DMT, without the need to follow a proper pKa curve. I know its nice when you have more experience and want to experiment with chemistry and be exact, but for most people this is not really important.

For the OP: Yeah excess lye is no problem, also it further breaks down bark and will prevent emulsion. The only thing is that it might be a waste of material, as you already know

 

[benzyme]

significant? maybe not significant, although excessive anion concentration will certainly oxidize the product. this is nothing new, it's fundamental chemistry.
and pure dmt from STB? where is the data? I've seen lots of pics, but no measurements (and I'm not talking about weight). all these 1 and 2% claims are very suspect.

1:1 is a huge waste, sloppy chemistry.
physical methods can do a more efficient cell lysis, so you can employ a more efficient basification. 13.0 - 13.2 gives 99.96 to 99.97% free base, respectively, and this gradually decreases as the pH increases. 14 is overkill. just sayin'

 

[Electric Kool-Aid]

Cant we all just get a bong???


Sorry couldnt resist!! hehe

 

[jayjay001]

Oh, I had a question about this. How does the ratio of water to lye affect the pH of the substance?

I just thought it was odd that the instructions for noman's tek suggest more water for powdered MHRB but not more lye or more naptha.

Is it the ratio of lye to MHRB or lye to water that matters? I was assuming it was lye to water, since that's what's being used to break down the bark... and I thought it was strange that no comments were made on anything but increase in water, but I figured that so many people have been using the tech with success that I shouldn't worry about it.

 

[benzyme]

lye has a specific solubility in water; some people think, for whatever misguided reason, that using a lot of lye with less water is more efficient since it's less liquid to work with

 

[endlessness]

significant? maybe not significant, although excessive anion concentration will certainly oxidize the product. this is nothing new, it's fundamental chemistry.
and pure dmt from STB? where is the data? I've seen lots of pics, but no measurements (and I'm not talking about weight). all these 1 and 2% claims are very suspect.

1:1 is a huge waste, sloppy chemistry.
physical methods can do a more efficient cell lysis, so you can employ a more efficient basification. 13.0 - 13.2 gives 99.96 to 99.97% free base, respectively, and this gradually decreases as the pH increases. 14 is overkill. just sayin'

Instead of saying its fundamental chemistry (or theory of it..) , please show a mass spec of oxidation products of DMT extracted with excess NaOH... I have never heard or seen such thing, though theory sounds fine....

Reasonably pure DMT from STB yes, even without recrystallization. Ive posted some of it in the analysis thread.. Some more LC work soon to come. I doubt me, you or anybody else would notice the difference when smoking that from smoking some DMT purified by column work, in a blind test, so I dont see your point and I think its nitpicking.

I dont disagree its a waste to use a lot of NaOH in STB, personally thats not my way of extracting, but appart from the simple fact that there's a lot of NaOH, there's no real issue there imo.

Not everyone has a sonicator (or a pressure cooker).

I think its fine saying your opinion and suggesting other possible methods, it can help people learn and rethink and try to be more efficient. but I think its important to also be careful with coming with a ready speech and some advanced vocabulary, but realize who you are answering to, if the answer is adequate to the question asked and adjusted to the chemistry level of the person.. No offense, always glad for your feedback around the forums

Jayjay, forget the suggestion for more water for powdered MHRB, the original ratio works perfectly fine.

and yes, the more lye (or hydroxide ions) to water ratio, the higher the pH. But pH is also logarithmic scale, meaning each pH point increased means its 10x more basic (or 10x more acidic if it lowers) than the previous point.

Im not sure what pH it would be in the recommended extra water noman version, but considering the original ratio is already using excess lye, I think whatever pH decrease, it will still be high enough pH.

Ratio of MHRB to lye also matters because part of the lye will be used to neutralize the acids in the mimosa.. So yeah its a factor of all of those things.

Use the tek without extra water and indeed dont worry about it. And yeah for the future you can research other ways like more efficient A/Bs and so on.

 

[jayjay001]

Just to note, I really appreciate all the information! I love it when people are informed on a subject and are willing to take the time to share what they know, I really don't care how you come across.

Now I'm curious as to what the ideal ratio of lye to water would be to avoid excessive pH. I'm far more concerned with a higher purity of DMT than I am in saving lye.

I'm not all that great with chemistry so I'd trust someone who at least sounds like they know what they're talking about...

*EDIT* Oh hey, just found a neat online pH calculator

http://www.sensorex.com/support/more/ph_calculator

It suggests that 4g of sodium hydroxide mixed with 750ml of water (the amount of water for 50g of MHRB in noman's tek recomended originally) yields a 13.12 pH solution.

Can anyone support this as a good idea? or vice versa?

*/EDIT*

 

[endlessness]

jayjay, the thing is that there are other variables at play. First of all, as soon as mimosa is in that water, it will lower the pH.. Also, the other thing is, the extra lye will probably help your yield, unless of course if you do an A/B, then you need much less. In any case the neat thing about mimosa is that it has its "internal pH indicator", so-to-speak, which is that once it reaches around pH 13, it turns jet black. So just add lye till its all black, and that should be enough (you'll see it will be a lot less than the tek asks for), or you can add a bit more for good measure. When mixing the layers, stir it, dont shake, otherwise you might have emulsions (more lye diminishes chances of emulsions, which specially with STBs are a problem). In any case if you get emulsions, check the FAQ for solutions, it can be solved.

Also as you pull the alkaloids out, the pH will lower a bit, so later pulls have more chance of emulsion ime.. You can add a bit more lye after a couple of pulls.

 

[benzyme]

Instead of saying its fundamental chemistry (or theory of it..) , please show a mass spec of oxidation products of DMT extracted with excess NaOH...

haha, that's my shtick, you can't steal it; you're saying it to someone who cut his teeth on LC-MS for the last couple years. you guys theorize with plates that some n-oxide is present, but don't reproduce it with GC-MS. i'm merely proposing a possible reason for the presence of this supposed oxide. my extractions never showed an n-oxide in the spectra, but i'm fairly meticulous and measure pH.

and yes, the more lye (or hydroxide ions) to water ratio, the higher the pH. But pH is also logarithmic scale, meaning each pH point increased means its 10x more basic (or 10x more acidic if it lowers) than the previous point.
.

you're not mentioning the solubility factor; NaOH requires a certain amount of water for dissociation to occur,
your theory doesn't hold at low volumes of water, as much of the base will still be in solid phase

 

[endlessness]

haha, that's my shtick, you can't steal it; you're saying it to someone who cut his teeth on LC-MS for the last couple years. you guys theorize with plates that some n-oxide is present, but don't reproduce it with GC-MS. i'm merely proposing a possible reason for the presence of this supposed oxide. my extractions never showed an n-oxide in the spectra, but i'm fairly meticulous and measure pH.

My point is that, you came to the thread saying that excess OH causes oxidation (implying it is in a significant degree that would matter to any normal home chemist reading this thread, no?). I ask for evidence because I havent seen much, and if you say with so much certainty that it occurs significantly, then I supposed you might have seen it. But you say you are meticulous, and never seen it, which isnt really evidence for those not being meticulous and therefore the 'significant oxidation' due to -OH is an evidenceless theory so far at least when talking about DMT oxidation. Anyways this can be answered in the soon future so we just wait

you're not mentioning the solubility factor; NaOH requires a certain amount of water for dissociation to occur,
your theory doesn't hold at low volumes of water, as much of the base will still be in solid phase

I thought that was a given... Definitely there's always a limit of solubility. But the ratios used in STBs are still quite far from that

 

[benzyme]

my point initially was that it's really excessive to use that much base,
i never said 'significant' oxidation occurs. it's mainly just a waste of base

 

[geko42]

Thank you all for your opinions and insight, it has been invaluable in drawing my own opinions.

swim does agree it may be a waste of materials, but 1:1 seams to be working well for now.