Minimum Polymer

[IridiumAndLace]

As for my batch, I think I might start with the tea, since it's the most accessible. My pulls were always just putting the heptane with the tea into a 2L Erlenmeyer flask, and putting it on the stirrer for a couple hours. Maybe some good hard shaking will help?

This feels plausible... When I did my little mini-A/B on the heptane from my first pull, I had to shake it hard and let it separate multiple times before the liquid turned clear--in both directions. Perhaps I'll try a pull like that next, just to see if a lot of agitation makes a difference.

Update: Extensive agitation did produce some additional product, but like the first batch, it came with a lot of that annoying uncrystallized spice, and the resulting scraping was also brown and crunchy.

End result from my pressure cooker batch:

•First pull (w/ 190ml clean heptane): 0.318g, nasty, orange, crunchy, did not want to crystallize
•Second pull (w/ 50ml used heptane): 0.024, reasonably white
•Third pull (w/ 100ml used heptane and heavy stirring): 0.129g, brown and crunchy
•"Bonus" pull, when I did a mini-A/B on the heptane from the first pull: 0.074g, fairly white w/ some yellow oxidation

Total: 0.545g of rough, contaminated spice, 1.09% yield. Gonna need to re-x this, hopefully won't require a mini-A/B to get my usual fluffy white xtals.

All in all, I'm afraid I have to call this a failure in that it did not improve either my yield or the quality of my product versus a standard A/B with citric acid. There might be more spice still locked up in the solids or in the tea in some form that heptane can't extract, but at this point I've been fussing with this extraction for a week and I'm kind of over it and ready to move on.

For my next run, I'll try the latest update to the minimum polymer tek, using ascorbic acid and extra water as indicated. Once the cooking is done, I'll filter the resulting tea and basify/pull from the tea and solids separately, to see if there remains any meaningful amount of spice in the plant matter. I'll report back soon...

 

[IridiumAndLace]

Speaking of the tek @Loveall, did you mean to edit it so that you're PCing in plain (neutral) water and only acidfiying after cooking? I'm wondering what the theory is there?

 

[Loveall]

Speaking of the tek @Loveall, did you mean to edit it so that you're PCing in plain (neutral) water and only acidfiying after cooking? I'm wondering what the theory is there?

Yes, I learned that ascorbic acid degrades after 160F, so moved to using it after pressure cooking.

However, perhaps it is better to adjust pH to 4 before pressure cooking like Northerner did. With plain water, the bark is already slightly acidic on it's own (pH ~ 5). I wanted to see if the ascorbic acid treatment is what really minimized goo, but it would be also a good test to adjust pH to 4 with vinegar or citric acid before PCing.

- PC step: cell lysing and DMT extraction into water
- 8 hour warm ascorbic acid treatment: DMT de-polymerization

The solvent step also seems important to minimize new goo formation. Boiling with fresh solvent after freeze precipitation and evaporating at room temperature (instead of freezing again) seems to help.

 

[IridiumAndLace]

Ohhh, good call on the ascorbic acid. It didn't occur to me that it's not heat stable... Now it's got me thinking, does citric acid degrade at high temperature? [Edit: Only at around 160°C, quite a bit hotter than a pressure cooker.]

Ok, I have to think our choice of solvent has something to do with this. I've always found that evapping solvent--either acetone or heptane--produces that clear, sticky, oily "goo" that coats the bottom of the container. Scraping crystals through it causes it to harden, otherwise it'll crystallize spontaneously into frostlike xtals in about a week. That's not the "polymer" you're referring to, is it?

Anyway, ok. I'll try another run this evening: 50g MHRB with just a small dash of citric acid (pH 4, you think?) in 750ml of water for four hours in the pressure cooker. Once it comes out of the PC I'll acidify with ascorbic acid and let it stir on the hot plate set to 60°C overnight. Then tomorrow I'll pull with clean heptane and see what I get.

 

[Loveall]

Ohhh, good call on the ascorbic acid. It didn't occur to me that it's not heat stable... Now it's got me thinking, does citric acid degrade at high temperature? [Edit: Only at around 160°C, quite a bit hotter than a pressure cooker.]

Ok, I have to think our choice of solvent has something to do with this. I've always found that evapping solvent--either acetone or heptane--produces that clear, sticky, oily "goo" that coats the bottom of the container. Scraping crystals through it causes it to harden, otherwise it'll crystallize spontaneously into frostlike xtals in about a week. That's not the "polymer" you're referring to, is it?

Anyway, ok. I'll try another run this evening: 50g MHRB with just a small dash of citric acid (pH 4, you think?) in 750ml of water for four hours in the pressure cooker. Once it comes out of the PC I'll acidify with ascorbic acid and let it stir on the hot plate set to 60°C overnight. Then tomorrow I'll pull with clean heptane and see what I get.

Yes, hypothesis is that goo that can go back to harder crystals is part of the polymers we are talking about. There seems to be lots of ways to get polymers. Everything seems to matter, including the solvent used.

I think DMT just likes to stick to itself and will do so if it gets a chance. Some of it may also come aggregated like that from the plant. It is possible that the solvent treatment undoes some of the vitamins C work, so the details of what is used may be super important. Time in hot naphtha seems to help de-polymerization.

I'm using VM&P naphtha. It is a mix of C5-C10 saturated hydrocarbons. I know it boils at 115C.

Citric acid should be fine in the PC (~400K). It is stable at that temperature. pH 4 makes sense since that is what Northerner did for his excellent result (but not sure what specific acid he used).

 

[Loveall]

Ok, results from 50g MHRB, 4 hour PC (in jar) + 8h Vitamin C 155F treatment are 1st picture: 4 pulls done and freeze precipitated (first pull top left had a little yellow throughout). Had some goo, but I consider it minimal/small. 2.3% yield (590mg + 360mg + 170mg + 30mg). Pulls were done with used naphtha and no pre-evaporation. Overall I'm happy with the result and like this process. I'm not gonna claim it is better than max ion in general, personally I think I got a record low point of goo for this bark, but the difference is not huge.

I dissolved the pullls in a small amount of hot naphtha. As that cooled, a small amount of red goo precipitated first, at which point I decanted off the solution and let it evaporate. The result from evaporation were shiny white xtals which scraped up to a pretty white (second picture). That was 1g of DMT (2% yield). Note that I never get shiny when freeze precipitating, it could be that evaporation forms a nice structure that is different from freezing.

Now for the small amount of red dots which I think is DMT goo. I'm trying different solvents to break it up. Got an interesting result when using acetone + limonene, goo went from red to orange (but not xtals yet) - I think that means the goo was broken down some but not completely. Benzyme was able to completely break up red goo using petroleum ether (which I think is simply low boiling point naphtha). My painters naphtha is heavier than that (wont boil on a boiling water bath), perhaps that makes a big difference.

What I think I have learned (could be wrong):

- A long intial acid treatment seems to break down natural bark goo. Ascorbic acid does a good job. Other acids seem to help also. Note the max ion has an 8 hour warm acid treatment of the bark with natural enzymes intact, I think this is a very important step that breaks down DMT polymer. Advantage of doing this early is to improve the partion coefficient into naphtha.
- Gentle basing conditions keep goo at bay
- The solvent is very important. Gonna try to get a hold of petroleum ether somehow. Painters naptha (heavier, longer C chains) which I have been using may not be able to break down DMT polymer. Testing with other solvents may be a good idea (e.g. methanol) - see if something can really dissolve DMT polymer at the very end and give xtals.

 

[Loveall]

Ok, so experimentally lighter naphtha (e.g. camping fuel) is better for minimum polymer. It seems to break up DMT polymer when boiling much better than heavy naphtha (paint thinner) when hot.

Lighter naphtha has been recommended before, this is not something new in general. I think the claim that hot light naphtha breaks up DMT goo better than heavy naphtha is a new potential learning (at least for me).

Attaching the MSDS of the solvent I'm moving to for minimum polymer experiments. Hoping that when everything is done together (long heated acid step + gentle basing), DMT polymer is indeed kept under control through the whole process

 

[IridiumAndLace]

Ok, results from 50g MHRB, 4 hour PC (in jar) + 8h Vitamin C 155F treatment are 1st picture: 4 pulls done and freeze precipitated (first pull top left had a little yellow throughout). Had some goo, but I consider it minimal/small. 2.3% yield (590mg + 360mg + 170mg + 30mg). Pulls were done with used naphtha and no pre-evaporation. Overall I'm happy with the result and like this process. I'm not gonna claim it is better than max ion in general, personally I think I got a record low point of goo for this bark, but the difference is not huge.

*Raises hand* Question! How much NPS did you use for each pull?

 

[Loveall]

Ok, results from 50g MHRB, 4 hour PC (in jar) + 8h Vitamin C 155F treatment are 1st picture: 4 pulls done and freeze precipitated (first pull top left had a little yellow throughout). Had some goo, but I consider it minimal/small. 2.3% yield (590mg + 360mg + 170mg + 30mg). Pulls were done with used naphtha and no pre-evaporation. Overall I'm happy with the result and like this process. I'm not gonna claim it is better than max ion in general, personally I think I got a record low point of goo for this bark, but the difference is not huge.

*Raises hand* Question! How much NPS did you use for each pull?

It was about 65ml. I used a scale to measure (50g of naphtha).

 

[IridiumAndLace]

I've been running through a slight variation of your most recent test, trying to replicate your results. As I'm looking at the MHRB solids I filtered out, I got to thinking... Has anyone ever attempted lysing the MHRB using strong base in the pressure cooker?

Real danger alert: Sodium hydroxide attacks metals, especially aluminum. This would have to be done in open glass containers in the pressure cooker. Attempting to PC sodium hydroxide directly in a metal pressure cooker could damage the cooker and cause it to fail, explosively.

My hypothesis is that since basifying MHRB powder under STP turns it into a grainy gelatinous mess, maybe basifying it under high temperature and pressure would dissolve the plant matter altogether. What better way to liberate the DMT from the plant material than to cause it to stop being plant material?

Once it comes out of the pressure cooker, the initial round of NaOH would be neutralized to pH 7 with acetic and/or citric acid. The brew would then be aggressively acidified with ascorbic acid, cooked low and slow for 8 hours to break up any DMT polymer, followed by gentle basifying and pulling.

Thoughts? Is it worth trying?

 

[Loveall]

I've been running through a slight variation of your most recent test, trying to replicate your results. As I'm looking at the MHRB solids I filtered out, I got to thinking... Has anyone ever attempted lysing the MHRB using strong base in the pressure cooker?

Real danger alert: Sodium hydroxide attacks metals, especially aluminum. This would have to be done in open glass containers in the pressure cooker. Attempting to PC sodium hydroxide directly in a metal pressure cooker could damage the cooker and cause it to fail, explosively.

My hypothesis is that since basifying MHRB powder under STP turns it into a grainy gelatinous mess, maybe basifying it under high temperature and pressure would dissolve the plant matter altogether. What better way to liberate the DMT from the plant material than to cause it to stop being plant material?

Once it comes out of the pressure cooker, the initial round of NaOH would be neutralized to pH 7 with acetic and/or citric acid. The brew would then be aggressively acidified with ascorbic acid, cooked low and slow for 8 hours to break up any DMT polymer, followed by gentle basifying and pulling.

Thoughts? Is it worth trying?

I wouldn't do it. NaOH can attack glass at high temp and pressure. Even if using borosilicate glass, it could boil out of the container and get to the metal.

I think the plant material is well Lysed. If you want to do more, you can freeze/thaw 3x, an then gentle-acid pressure cook on top of that.

 

[Jees]

I keep thinking bark potency is key in this, if one follows a tek to the T.

How much is there to win by doing agressieve things? It would be interesting to know but in any case it would not be recommendable to make it into a habitual routine, sooner or later things go south, Murphy's law.

One notch lesser dangerous than boiling caustic might be throwing bark as powdered fines in well ventilated room temp muriatic acid or so as a primary step?

I subscribe the forum stance on safety-first, nevertheless had some basified soup flying around against my will, all good in the end but things could have been worse, knock on wood.

 

[Loveall]

The lighter naphtha made a big difference.

I combined it with a long hot vitamin C treatment and I really like what I got.

Also, wanted to keep the plant enzymes active, so I did not pressure cook.

So far this is the beast combo for (hypothetical) min polymer I have found.

1) 50g of bark + 700ml of water, 3x freeze/defrost.
2) ~10g of vitamin C, heat to 150F in pot with lid, and keep at this temp for a long time (8+ hours). In this experiment I inadvertently got it to a boil after a few hours which made the color a dark red and could have destroyed the vitamin C and plant enzymes. I lowered the temp to 150F and added 5g of fresh vitamin C and kept it like that for 12 hours. Next time I'll stay at 150F for the entirety of the extraction. Interestingly, this made a very light red color return to the brew.
3) Transferred to a mason jar (including bark, no filtering) and added water to about an inch of the top. Added the light naphtha (Coleman camping fuel) and them based. Was shooting for ~25g of lye, but a clump of NaOH fell in and I got 37g of lye.
4) After warm heated pulling and feeze precipitation prodt DMT I have ever seen. Yield looks great too (eyeballing), I expect no issues there. I'm talking snow white here.

I think that to really get min polymer all the steps need to work together. For example, if the basing step is too aggressive, DMT will (re)polymerize and the naphtha type won't matter as much. Or if the natural DMT is not polymerized completely, you will get yellow DMT at the end even with gentle basing and light naphtha. Etc. Again, no hard proof, but experimentally the hypothesis fits so far.

I'll keep on working on this, but I think focusing on min polymer techniques could help get consistent white product, and minimize goo. Doesn't matter for torch, but for e-mesh and complexation it may give more consistent results.

 

[Loveall]

So there are some questions about Coleman fuel having rust prevention additives not mentioned in their MSDS.

I'm doing a larger evaporation test to make sure it stays clean.

The DMT xtals are very white and look great, but need to make sure the source of light naphtha is not an issue - FYI.

 

[Jees]

Keep going

...3) Transferred to a mason jar (including bark, no filtering) and added water to about an inch of the top...

Just for the sake of wanking numbers, wether this matters or not, what kind of volume please? Mason jars come in different sizes where I live.
Thanks :thumb_up:

 

[Loveall]

Keep going

...3) Transferred to a mason jar (including bark, no filtering) and added water to about an inch of the top...

Just for the sake of wanking numbers, wether this matters or not, what kind of volume please? Mason jars come in different sizes where I live.
Thanks :thumb_up:

It's a quart jar.

I think I found a less questionable source of light hydrocarbons where I live: ronsonol lighter fluid. Cyb and others mention it in the forum as reliable, colorless, and having clean evaporation.

 

[IridiumAndLace]

Also, wanted to keep the plant enzymes active, so I did not pressure cook.

I've been following your tests myself as closely as I can... It's hard to draw firm conclusions since I'm changing several variables at once (different bark, filtering, pulling with heptane). But, after two batches in the pressure cooker, I'm finding my already-low yields are maybe half what I normally get from a Max Ion Tek extraction. I'm becoming convinced that the pressure cooker is either destroying the DMT, or rendering it into a form that can't be readily extracted by normal A/B tek methods.

Since my MHRB is already 3x frozen (I keep it in the freezer), I'll try your latest tek next. It looks pretty identical to a typical A/B tek at this point, no? Just using ascorbic acid in particular, low and slow acid cook, gentle basing, and pulling with good NPS. Essentially what I was doing previously with, well, better results than I'm getting now.

...Doesn't Coleman Camp Fuel contain a blue dye? Or am I thinking of something else? Conversely, I'd love to see your result doing the same tek on the same bark, but pulling with Bestine.

So there are some questions about Coleman fuel having rust prevention additives not mentioned in their MSDS.

Heh. I picked up a quart of Coleman fuel this afternoon, before I saw this. Glad I didn't get the gallon instead! Did you ever do that evap test?

I think I found a less questionable source of light hydrocarbons where I live: ronsonol lighter fluid. Cyb and others mention it in the forum as reliable, colorless, and having clean evaporation.

Also known as Zippo fluid? A cursory Google search suggests it's the same exact product in both bottles.

 

[Loveall]

Also, wanted to keep the plant enzymes active, so I did not pressure cook.

I've been following your tests myself as closely as I can... It's hard to draw firm conclusions since I'm changing several variables at once (different bark, filtering, pulling with heptane). But, after two batches in the pressure cooker, I'm finding my already-low yields are maybe half what I normally get from a Max Ion Tek extraction. I'm becoming convinced that the pressure cooker is either destroying the DMT, or rendering it into a form that can't be readily extracted by normal A/B tek methods.

Since my MHRB is already 3x frozen (I keep it in the freezer), I'll try your latest tek next. It looks pretty identical to a typical A/B tek at this point, no? Just using ascorbic acid in particular, low and slow acid cook, gentle basing, and pulling with good NPS. Essentially what I was doing previously with, well, better results than I'm getting now.

...Doesn't Coleman Camp Fuel contain a blue dye? Or am I thinking of something else? Conversely, I'd love to see your result doing the same tek on the same bark, but pulling with Bestine.

So there are some questions about Coleman fuel having rust prevention additives not mentioned in their MSDS.

Heh. I picked up a quart of Coleman fuel this afternoon, before I saw this. Glad I didn't get the gallon instead! Did you ever do that evap test?

I think I found a less questionable source of light hydrocarbons where I live: ronsonol lighter fluid. Cyb and others mention it in the forum as reliable, colorless, and having clean evaporation.

Also known as Zippo fluid? A cursory Google search suggests it's the same exact product in both bottles.

After more evap tests with larger volumes, avoid Coleman. There is a die in there. Sorry I mentioned it, the SDS threw me off. There are old threads on the nexus about this too, and blue DMT is indeed am issue with this solvent. My bad.

Yes, the approach has been converging towards Cyb's max ion tek. The differences focus on min-polymer:

- 8+ hour acid soak: Vit C at 150F instead of warm vinegar or citric acid.
- Solvent: Use the lightest naphtha available. Smaller hydrocarbons seem to disrupt DMT aggregation based on separate tests on goo. This is also mentioned in older nexus threads and not new (but I was not aware of how important it is, makes a big difference). I've been using heavier painters naphtha for years, but no more.
- Pulls: Shake in naphtha before basing. Keep NaOH concentration low inside the lower-limit boundary condition that the emulsion breaks up. Skip adding salt and do lot let the based extract sit for 2 hours. Higher pH than needed, higher ionic strengh, and time in base are all conducive to DMT aggregation. The good partition coefficient for min-polymer comes from having DMT that is not aggregated (increased solubility in naphtha) instead of salting out (decreased solubility in water).
- Freeze precipate: Before freezing, heat the combined pulls in a hot water bath for ~30 minutes. See if you can get the solvent to boil (a good sign that light naphtha was used). This heat treatment befor freezing can break down DMT agregates. This step may be overkill if the previous steps did their job at minimizing polymer.

About the last bullet: It could be that following max ion with two small updates makes a hybrid max ion/min polymer. Simply follow max ion with two caveats: 1) insist on low count C chain light naphtha, and 2) heat/boil the pulls before freeze precipitation.

I've also heard that Zippo lighter fuel is same/similar to ronsonol. When I checked the SDS I saw that:

- Ronsonol is 70% Light Hydrotreated Distillate (CAS #68410-97-9) and 30% Hydrotreated Light Naphtha (CAS #64742-49-0). It does say it is manufactured by Zippo.
- Zippo is 50-100% Light Hydrotreated Distillate (CAS #68410-97-9) and 25-50% Hydrotreated Light Naphtha (CAS #64742-49-0), boiling point >35C.

So they could be similar/identical. A boiling test could inform if one is lighter (whichever boils first if ther is a difference). I can say that I'm getting very good results with Ronsonol (seen at Ace hardware and Walmart).

 

[Dirty T]

I recently tried a different approach where I added the bark to the basified water then immediately added 60g salt and 50ml hot Naphtha before shaking and it resulted it pure white crystals and very decent yield. 1% on first pull. I've noticed keeping everything hot and adding salt really keeps the goo away and when I do get goo on yhe later pulls it is just a layer between all the crystals.

I honestly don't mind goo mixed with crystals though, it isn't any more difficult to me to ingest by vaporization. I do find this thread fascinating and have found myself getting the biggest white crystals possible short of AB or backsalting. Does anyone have an explanation to why backsalted freebase crystals are shiny and DMT that has not been converted back and forth is not? I want to learn as much about the molecule as I can.

 

[Loveall]

I recently tried a different approach where I added the bark to the basified water then immediately added 60g salt and 50ml hot Naphtha before shaking and it resulted it pure white crystals and very decent yield. 1% on first pull. I've noticed keeping everything hot and adding salt really keeps the goo away and when I do get goo on yhe later pulls it is just a layer between all the crystals.

I honestly don't mind goo mixed with crystals though, it isn't any more difficult to me to ingest by vaporization. I do find this thread fascinating and have found myself getting the biggest white crystals possible short of AB or backsalting. Does anyone have an explanation to why backsalted freebase crystals are shiny and DMT that has not been converted back and forth is not? I want to learn as much about the molecule as I can.

Interesting. Which brand naphtha did you use? How hot was the Naphtha/water? How much bark and how much water? Thanks.