Minimum Polymer

[Dirty T]

Kleen Strip VM&P, 800ml water, 50 grams MHRB (powdered using an Amazon 'mechanical root grinder" it results 8n powder and pencil shaving sized bits) 60 grams WinCo brand Non-Iodized salt, 50ml Naphtha (60* Celsius on hot plate) in 1 quart mason jar (I've noticed the 'factory' lids are fairly resistant to Naphtha and Lye but Xylene trashes them. I recommend new lids for every extraction just to be safe). I should also state here I always start with recycled Naphtha so it has a yellow tint before I start but that does not translate to colored crystals. I get better yields this way than fresh Naphtha. I only clean Naphtha after I backsalt to remove any residual fumaric or citric acid and prevent cloudiness. I haven't had cloudy solvent yet that couldn't be cleaned with a sodium carbonate wash or two.

I think the backsalt process is my favorite part of extracting MHRB. I love watching Xylene crash crystals into the acidic solution. I should also state I use the same process for Xylene pulls with heat, except at 80* rather than 60* and I always pull white crystals from "spent" bark (literally no more freeze precipation on pull with pre 'freeze temperature DMT saturated" Naphtha). Last time I also got a large cluster of orange crystals that Naphtha would not pick up, I pulled with Xylene and evaporated for nearly a gram of active goo after getting 2 grams of white crystals. I would say this goo is every bit as active as the crystals and once I folded it with crystals it's as easy to handle.

Don't toss that spent soup!

 

[IridiumAndLace]

Ok, I have final-ish results from my first three Minimum Polymer tests, each using 50g of powdered MHRB, filtering between the acid cook and basing steps.

My first run was with two gentle citric acid cooks, and basifying slowly under heptane. This resulted in a crude yield of 0.715g (1.43%), about the most I've gotten out of this MHRB. The product was fairly white, and seemed to get dirtier with each subsequent pull.

The second run was done with strong citric acid solution, in the pressure cooker. The crude yield was 0.531g, or 1.06%, of very rough crunchy yellow/orange/brown product. Lots of "goo", this seemed to produce the opposite effect we were going for.

The third run was identical to the second, except I used much less acid in the pressure cooker (only 5g of citric acid to 800ml of water). Pulling with 100ml of fresh heptane, I got 0.422g from the first pull and 0.124g from the second pull, both reasonably clean off-white product. I figure I had another 0.2g of DMT that didn't crystallize in the freezer and went into my used heptane bottle. This would give an approximate yield of 0.75g, not bad at 1.5%.

After these two pulls, I re-added the MHRB powder into the basified tea broth and did a couple more 50ml pulls. These yielded some yellow sludge that didn't form solid crystals in the freezer and could only be partially decanted. I'll evap it down and then do a mini-A/B on it to see if there's a meaningful amount of spice in it. It sure doesn't look like it, and I'm thoroughly convinced that I'm not losing a meaningful amount of spice by filtering my tea before basifying.

(Also, I was reminded once again why I never, ever put basified MHRB solids into my separatory funnel. Fishing a wire through the neck of my sep funnel to try and clear the clogged stopcock really makes a person question their life decisions, y'know?)

I combined the first two runs for a single recrystallization. The result from the freeze precip is attached; the re-x produced lots of white crystals, sticking up out of a solid layer of hard yellow stuff ("goo" ), which is not normal for me. I gently scraped the xtals off the top, and got 0.567g of my usual beautiful sparkling white product. I then scraped the rest of the product off the dish, and got 0.621g of hard, dense, straw-colored powder. And, whereas my white xtals have only a faint floral DMT smell, the yellow product smells strongly like... well, burned DMT.

I figure I'll do a mini-A/B with ascorbic acid on this straw-colored product, and see if I can clean it up. A good question occurred to me:

How do I know if what I have here is:
a) Polymerized DMT or other DMT oligomers/polymorphs
b) DMT oxide and other breakdown products
c) DMT contaminated with plant fats or other jimjam
d) Something else??

...I suppose the mini-A/B will at least answer the polymer question, if indeed our hypothesis that ascorbic acid breaks down DMT polymer is true. I'll report results back soon.

 

[Loveall]

The yellow goo could be a new form of DMT aggregation as we fumble to figure out de-polymerization.

Which solvent are you using? Turns out this could be very important.

How do I know if what I have here is:
a) Polymerized DMT or other DMT oligomers/polymorphs
b) DMT oxide and other breakdown products
c) DMT contaminated with plant fats or other jimjam
d) Something else??

I think trying to convert it to xtals is easiest to see if it is indeed DMT. Analysis would be best, but not always easily available. I guess heating is another option, DMT oxide reportedly doesn't vaporize well (see this). DMT oxide is unlikely to be in our extractions I believe.

Plant oils are unlikely I believe. As a check, once I did an acid defat and freeze precipitation and got nothing. I think oils shouldn't care if they are being pulled from an acid or a base.

My guess is that the yellow stuff is DMT that is partially de-polymerized. Could be new for you since we are trying to (in theory) de-polymerize it. Just a guess on my part.

 

[Loveall]

Kleen Strip VM&P, 800ml water, 50 grams MHRB (powdered using an Amazon 'mechanical root grinder" it results 8n powder and pencil shaving sized bits) 60 grams WinCo brand Non-Iodized salt, 50ml Naphtha (60* Celsius on hot plate) in 1 quart mason jar (I've noticed the 'factory' lids are fairly resistant to Naphtha and Lye but Xylene trashes them. I recommend new lids for every extraction just to be safe). I should also state here I always start with recycled Naphtha so it has a yellow tint before I start but that does not translate to colored crystals. I get better yields this way than fresh Naphtha. I only clean Naphtha after I backsalt to remove any residual fumaric or citric acid and prevent cloudiness. I haven't had cloudy solvent yet that couldn't be cleaned with a sodium carbonate wash or two.

I think the backsalt process is my favorite part of extracting MHRB. I love watching Xylene crash crystals into the acidic solution. I should also state I use the same process for Xylene pulls with heat, except at 80* rather than 60* and I always pull white crystals from "spent" bark (literally no more freeze precipation on pull with pre 'freeze temperature DMT saturated" Naphtha). Last time I also got a large cluster of orange crystals that Naphtha would not pick up, I pulled with Xylene and evaporated for nearly a gram of active goo after getting 2 grams of white crystals. I would say this goo is every bit as active as the crystals and once I folded it with crystals it's as easy to handle.

Don't toss that spent soup!

So you get 3g of DMT from 50g? That's 6%. Maybe you meant 100g of DMT in the second paragraph.

That yield boost with xylene is cool. But perhaps, if DMT can be De-polymerized before pulling it can all move into light naphtha without having to reach for the xylene? Just a guess on my part.

 

[IridiumAndLace]

The yellow goo could be a new form of DMT aggregation as we fumble to figure out de-polymerization.

Which solvent are you using? Turns out this could be very important.

I'm pulling with purified heptane, or rather Bestine that I ran though a distillation column. I've noticed that it distills at 93°C, 5 degrees lower than the boiling point of n-heptane, so I suspect it's actually an azeotrope of heptane isomers. (I don't actually know if heptane forms an azeotrope with its own isomers, but that's my best guess. Otherwise, what is being sold as 99.9% pure heptane is actually mostly 3-ethylpentane. Either way, it seems to work great for extracting as white of xtals as I've ever seen.)

This yellow goo is very unusual for me, because I never got it prior to using the pressure cooker. It almost seems like the PC had the opposite effect, and actually caused my spice to polymerize more. Or, like I said, it liberated plant fats that I didn't used to have to deal with, and I'm now struggling to remove. What's strange is that my first pulls tend to be cleaner and whiter, and get smaller and dirtier as I go.

Regardless, I'm now pondering my next move for my mini-A/B. Should I dissolve this product back into a small amount of heptane, and then wash that with acid to get it into aqueous solution? Goal there is to eliminate nonpolars that don't form an ascorbate salt. Or should I just go straight to mixing it with water and seeing how much acid it takes to dissolve it all?

Maybe I'll do the latter, since I can calculate how much ascorbic acid it "should" take to turn all this into salt. Then I can filter off whatever doesn't dissolve. That seems like a more reliable way to separate nonpolar contaminants?

 

[Loveall]

The yellow goo could be a new form of DMT aggregation as we fumble to figure out de-polymerization.

Which solvent are you using? Turns out this could be very important.

I'm pulling with purified heptane, or rather Bestine that I ran though a distillation column. I've noticed that it distills at 93°C, 5 degrees lower than the boiling point of n-heptane, so I suspect it's actually an azeotrope of heptane isomers. (I don't actually know if heptane forms an azeotrope with its own isomers, but that's my best guess. Otherwise, what is being sold as 99.9% pure heptane is actually mostly 3-ethylpentane. Either way, it seems to work great for extracting as white of xtals as I've ever seen.)

This yellow goo is very unusual for me, because I never got it prior to using the pressure cooker. It almost seems like the PC had the opposite effect, and actually caused my spice to polymerize more. Or, like I said, it liberated plant fats that I didn't used to have to deal with, and I'm now struggling to remove. What's strange is that my first pulls tend to be cleaner and whiter, and get smaller and dirtier as I go.

Regardless, I'm now pondering my next move for my mini-A/B. Should I dissolve this product back into a small amount of heptane, and then wash that with acid to get it into aqueous solution? Goal there is to eliminate nonpolars that don't form an ascorbate salt. Or should I just go straight to mixing it with water and seeing how much acid it takes to dissolve it all?

Maybe I'll do the latter, since I can calculate how much ascorbic acid it "should" take to turn all this into salt. Then I can filter off whatever doesn't dissolve. That seems like a more reliable way to separate nonpolar contaminants?

Either sounds good. You can use a pH meter as you add a known amount of acid slowly to help with alkaloid titration. Works well for mescaline. Also, evap the acid pulls to see if there is any oil or not. I think you will find no oil, the yellow stuff looks like DMT to me.

I also think boiling in heptane for a while can turn the yellow stuff to xtals (if it is DMT). As the solvent heats up, the yellow stuff forms a separate layer at the bottom, then it eventually goes into the solvent with more heat. If you observe this, it would be very interesting: adding a solvent boil between pulling and freeze precipitation may help break up any remaining polymer from the plant extraction. I got partial conversion using heavier naphtha.

 

[Dirty T]

No I got 3g of DMT from 500g "spent" bark or more accurately the soup containing said bark. It seems no matter how long it sits there is always molecule left that Naphtha won't get but Xylene does (along with the fats, oils and trash) which is why I always backsalt when using Xylene and evaporate any residual Xylene on my scientific hot plate before I base and pull with Naphtha. Yes Xylene is harsh, toxic and probably as cancerous as gasoline, that's why I minimize it's use. Using it in my extractions has given me ideas to use it in other very practical ways.

My apologies if I lead you to believe I was getting 6% yield. I average 2.5% including Xylene pulls and backsalting the Naphtha once everything is completely drained.

 

[Loveall]

No I got 3g of DMT from 500g "spent" bark or more accurately the soup containing said bark. It seems no matter how long it sits there is always molecule left that Naphtha won't get but Xylene does (along with the fats, oils and trash) which is why I always backsalt when using Xylene and evaporate any residual Xylene on my scientific hot plate before I base and pull with Naphtha. Yes Xylene is harsh, toxic and probably as cancerous as gasoline, that's why I minimize it's use. Using it in my extractions has given me ideas to use it in other very practical ways.

My apologies if I lead you to believe I was getting 6% yield. I average 2.5% including Xylene pulls and backsalting the Naphtha once everything is completely drained.

Ah, so +0.6% from a xylene step on old spent basic bark soup, gotcha. Interesting, I may try that at some point.

 

[Jees]

Anecdotical goo story:

200ml pH 4 (vit C used) containing aprox 3 gr FB deems was 8 hours on 65degC.

At room temp started basing by dripping in saturated SodCarb solution on a stirrer, lot of gassing CO2, pH plateau started at pH9 (becoming cloudy) and milky at pH 9.4 but then got welcomed by a goo galore sticking on the glass and covering the pH elecktrode. A golden goo mess.
Added citric acid to drop to ph 4 to dissolve the goo mess successfuly.

This all hapened before any nonpolar was added, just illustrating firm goo forming in the watery phase, from milk to goo. Did I just exaggerate how-not-to? Looks like goo inducing circumstances.

I can imagine if a non polar would have been added and thus picking up the goo-potential, it would just crash goo out right before and during freezing. It leans toward having a goo engine in de basing phase.

 

[Dirty T]

I've tried all types of ways. My first extraction was in a stainless pot, I used a wood spoon and 400ml water, 200g lye, 200g powdered bark. I let it sit 24 hours then added Naphtha and stirred for 30 minutes then realized I can't see to pull it with a turkey baster so I poured it in a pickle jar and retrieved approximately 30ml of the 200ml Naphtha I had used, it had a wicked emulsion. I evaporated the Naphtha and got a small amount of goo I scrapped up and mixed with PG and put in a cartridge, the cartridge was a dud so I now transferred it again, vaped it all and got a headchange. My estimated yield was 5mg. That was all following a Tek I had read somewhere, I eventually remedied it and got about 1% or so. What a mess. Took me about 2 weeks to get it right.

 

[Loveall]

Anecdotical goo story:

200ml pH 4 (vit C used) containing aprox 3 gr FB deems was 8 hours on 65degC.

At room temp started basing by dripping in saturated SodCarb solution on a stirrer, lot of gassing CO2, pH plateau started at pH9 (becoming cloudy) and milky at pH 9.4 but then got welcomed by a goo galore sticking on the glass and covering the pH elecktrode. A golden goo mess.
Added citric acid to drop to ph 4 to dissolve the goo mess successfuly.

This all hapened before any nonpolar was added, just illustrating firm goo forming in the watery phase, from milk to goo. Did I just exaggerate how-not-to? Looks like goo inducing circumstances.

I can imagine if a non polar would have been added and thus picking up the goo-potential, it would just crash goo out right before and during freezing. It leans toward having a goo engine in de basing phase.

That is gentle pH. Why do you think goo formed so fast? Maybe 3g of DMT in 200ml is too concentrated? Pi-pi ring interactions happen when DMT comes close to itself, perhaps the concentration matters a lot. But people are successful with mini A/B? Could sodium carb be worse thank NaOH and induce goo?

 

[Jees]

...That is gentle pH...

Yes, was planning to up pH but I stopped as goo formed.

...Maybe 3g of DMT in 200ml is too concentrated? Pi-pi ring interactions happen when DMT comes close to itself, perhaps the concentration matters a lot...

The concentration was very high indeed. I choose about 15 to 20 mg/ml just too see if a pH depression occurs when the cloudynes sets in, simulating the situation where pH depressions occur with harmalas. No pH depression of any kind noticed with deems. A slight plateau was all, like a pH buffering effect, but no pH rollback at all.

...Could sodium carb be worse thank NaOH and induce goo?

Very likely since carbonates also gave me goo when crashing out harmalas with sodcarb (in those concentrations mentioned). Therefore (and other reasons) I preferred ammonia to avoid harmala goo.

Nevertheless I was surprised to see deems goo in the watery phase happening. This exaggerated situation learns something though, that there are potential goo mechanics in the watery base phase. Diluting might be a key here as you say, to be continued...

 

[Jees]

Same batch got upped volume to 1.5 liters (comes from 0.2 liters), added some citric acid and vinegar, 6 hours at 80 degC, cooled, based with again a lot of sodcarb to pH 9.8 (was hard to go higher with sodcarb) and no goo to see whatsoever! Modest amount of milk formed.

Added caustic to up pH to 11, most milk formed under this adding.

3 x 50ml Naphtha pulls at 50 degC and 4th pull at 60 degC, followed by 1x 100ml toluene pull for FASA.
Awaiting results.

 

[Jees]

Same batch got upped volume to 1.5 liters (comes from 0.2 liters)...Awaiting results.

So with everything near the same except volume rise, the cooling/freezing of the naphtha pulls happened without a trace of oil settling out at the bottom. Crystals were nice yellow but bone dry, very evenly across the tray, no spots of anything to notice.

Recuperated 1/3 of total yield as d-fumarate from FASA the last toluene pull. 2/3 of this came as white fine powder, the remaining 1/3 as hard goo?? See pic. Just at the spinner location only.
Because this dry crisping goo was so very locally hardened I tend to believe it was result of mechanical packing together by the spinner, hammering the floating particles.
I secretly fantasize it might have been the magnetical field of the spinner doing some woo wizardry on the fumarates

 

[Voidmatrix]

Hey all,

So, I did two more pulls from 2x100g MHRB from September or October (have been off lately) for a total of 4 pulls.

This was the result. Another 500mg+. 250mg+ from each soup.

I made sure to heat each soup jar for a couple hours before beginning pulling and the solvent was HOT as well.

Planning on doing at least another pull or two from each to see what happens.

These pulls were a little gooey, and there are a few dark goo flecks. I may re-x. On the other hand, I may also just use it for changa since I have plenty of freebase sitting around anyways.

One love

 

[Dirty T]

Looking pretty awesome there Voidmatrix. That looks like a nice pile of goodness there and that's a nice color for later pulls especially after sitting for a prolonged period. Very nice.

True story - I have a medical cannabis license so I store my DMT in a container labeled CBD isolate, looks nearly identical.

 

[Voidmatrix]

Looking pretty awesome there Voidmatrix. That looks like a nice pile of goodness there and that's a nice color for later pulls especially after sitting for a prolonged period. Very nice.

True story - I have a medical cannabis license so I store my DMT in a container labeled CBD isolate, looks nearly identical.

Right!?! I was pleasantly surprised! And thank you very much.

I'm thinking that heating each soup not only helped break up any emulsions there may have been, but also made the DMT more "available" for the solvent to "snatch" up as it was mixed through the soup. I've done subsequent pulls in the past, but have never gotten this much after.

I am kicking myself a little reflecting on the number of extractions that I did not do this, and thus, spice was wasted. But hey, we live and we learn right?

And that's awesome (the containers you use). I have become really fond of Infinity Jars. May order some more soon.

One love

 

[IridiumAndLace]

I also think boiling in heptane for a while can turn the yellow stuff to xtals (if it is DMT). As the solvent heats up, the yellow stuff forms a separate layer at the bottom, then it eventually goes into the solvent with more heat. If you observe this, it would be very interesting: adding a solvent boil between pulling and freeze precipitation may help break up any remaining polymer from the plant extraction. I got partial conversion using heavier naphtha.

Heh, I wish I had thought of this. I ended up doing the mini-a/b, using ascorbic acid.

I scraped up the goo and xtals into some chunky lumps, and added them to a solution of ascorbic acid. As the spice dissolved out, the lumps got softer and stickier, eventually turning into gooey globs stuck the inside of the flask. I discarded this sticky residue and proceeded to pull from the aqueous phase, yielding a very clean product. But looking back, you're right, I should have tried dissolving it into heptane and boiling it for a while. Oh well.

Along the same lines though, I had an idea to try a continuous liquid/liquid extraction. Not only could this theoretically extract every trace of available DMT from the tea, it would have the side effect of boiling the product in heptane for as long as the solvent is refluxing. I'm kind of excited to try this, once my glassware arrives....

 

[Ruffles]

Discovered something by accident, it may help people that are trying to manipulate the red oily stuff.

After FASA precipitating xylene derived NN-DMTs from MHRB (attention, this text is only fumaric stuff) we proceed into IPA cleanup stage, since there was a significant amount of reddish-yellowish gunk stuck to the walls of the glass recipient and scraping this was impossible. Dropping in warm IPA to redissolve what precipitated, the red-yellow gunk wouldn`t dissolve at all, even by boiling IPA it didn`t, white stuff did dissolve fully though. So the IPA was collected with whatever went into it for freeze precipitation (which came out white to light yellow).

The remaining red oily stuff was then dissolved in room temp 99% ethyl alcohol which became deep orange or light red after shaking and ressuspending it. This red EtOH was placed into the freezer overnight but only a small amount actually precipitated out of it (as red stuff). Placed 1:1 amount of IPA into the red EtOH (this was the accident) and it immediately turned cloudy at which point we realized we f@#$% mixed it up. So due to laziness we placed EtOH-IPA recipient into freezer overnight and lo and behold! Liquid was transparent and the red-orange gunk precipitated beautifully! Repeated this one more time with more red-orange EtOH and it worked again. Can`t really figure out why freezing EtOH or IPA by themselves doesn`t precipitate the orange red stuff while the combination does.

We usually dump the red fumaric stuff because it doesn`t really precipitate by IPA cleanup (only yellow to white drops out) and it complicates whatever drying procedure we try after FASA precipitation. It smells and tastes like normal white stuff does, a bioassay is due this weekend.

Due to this discussion we now have a lot of interest in the red hypothetical-polymer and if this IPA+EtOH precipitation of the red stuff is reproducible it may help whomever is trying to mess with it.

 

[IridiumAndLace]

So, here's a puzzler.

It seems like our description of "DMT polymer" is inching ever closer to our description of DMT oxide, with the exception that the polymerized DMT is soluble in NPS. Could it be that what we're actually fighting with is actually DMT oxide?

Per this thread, I did a little experiment as I was refining my latest crop of spice. I had off-white crystals, with some yellowey goo at the bottom of the dish. I took all my spice, dissolved it in a minimal amount of citric acid and water, and added a (large) excess of zinc powder. Attached is the progression of the results.

That's just after it was mixed, after a single shake, and after about 10 minutes of shaking. It didn't change visibly after that, and after an hour of heating and shaking I proceeded with decanting, basing, pulling, and freezing. It still needs one more re-x, but as of right now, I'm looking at the brightest, cleanest sparkling white xtals I've ever seen.

Maybe this yellow goo is DMT oxide. Maybe it's polymerized DMT. If someone really wanted to test this, I think you can make DMT oxide by dissolving DMT in acid and adding hydrogen peroxide. Then just do some solubility tests on the product, try treating it with zinc or a heptane boil, and see what happens.