Difference between revisions of "Chilled Acetone with IPA and Naphtha"

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(โ†’โ€ŽIntroduction ๐Ÿ™)
(โ†’โ€ŽConsumables๐Ÿ‘ฉโ€๐ŸŒพ)
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=Introduction ๐Ÿ™=
 
=Introduction ๐Ÿ™=
โˆ’
DMT free base manifestations, from white crystals to yellow powder to orange and even red goo, could be due to increasing degrees of aggregation<ref>Polymer MS evidence[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=88183]</ref> (see Fig. 1).
+
Pure DMT free base can form white crystals, yellow powder, and orange to red wax/goo. This wide range of appearance could be due to self aggregation because of indole ring pi bond stacking <ref>Polymer MS evidence[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=88183]</ref> (see Fig. 1).
  
  
โˆ’
This technique (TEK) focuses on manifesting plant DMT in its white crystalline form by minimizing DMT aggregation from both the plant and the extraction steps.
+
This technique (TEK) focuses on maximizing white crystalline DMT by minimizing self aggregation during extraction.
  
  
โˆ’
Thanks to benzyme for showing MS evidence of DMT weakly bonding to itself (pi stacking), and to Jees, downwardsfromzero, IridiumAndLace, and Loveall for their contributions to this process in the forum<ref>Minimum Polymer[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=97103]</ref>.
+
Thanks to benzyme for showing MS evidence of DMT weakly bonding to itself, and to Jees, downwardsfromzero, IridiumAndLace, and Loveall for their contributions to this process in the forum<ref>Minimum Polymer[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=97103]</ref>.
  
  
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* Water
 
* Water
 
* 50g of mimosa hostilis root bark
 
* 50g of mimosa hostilis root bark
โˆ’
* 10g ascorbic acid (vitamin C)
+
* 5g ascorbic acid
โˆ’
* ~250ml of '''very light naphtha''' (check SDS)
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* ~250ml of light hydrocarbonsโ€ 
 
* 25g of NaOH
 
* 25g of NaOH
 +
 +
 +
โ€ ''It is very important to use a source of light hydrocarbons. The smaller organic molecules seem to control DMT aggregation. Naptha used in paint applications tends to be too heavy. Petroleum distillate lighter fluids have molecules with smaller carbon chains and perform well (e.g. Ronsonol). Avoid products with anti rust or dies (e.g. Coleman camping fuel). Using the proper solvent is very important to control DMT aggregation if a white crystalline product is desired.''
  
 
==Equipment๐Ÿบ==
 
==Equipment๐Ÿบ==
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= Process Overview ๐Ÿ‘€ =
 
= Process Overview ๐Ÿ‘€ =
โˆ’
*Freeze/thaw bark 3x, treat with vitamin C at 150F for 8 hours, add <b>light</b> naphtha, basify gently, pull/boil/evaporate solvent, and freeze precipitate.
+
*Freeze/thaw bark 3x, treat with acid and CaCl2 150F for 8 hours, add light hydrocarbon solvent, basify gently with Ca(OH)2, pull/boil/evaporate/freeze solvent, decant/dry, scrape up.
  
 
= Detailed Process ๐Ÿ“œ=
 
= Detailed Process ๐Ÿ“œ=
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<center>''Fig. 2: Pressure cooked bark in quart jars.</center>
 
<center>''Fig. 2: Pressure cooked bark in quart jars.</center>
  
โˆ’
==Vitamin C Treatment ๐ŸŠ==
+
==De-polymerization==
โˆ’
Stir in vitamin C and gently heat to 150F. Cover pot with lid and keep jar at this temperature using very low heat for at least eight hours, keeping in mind that vitamin C begins to degrade at 158F.
+
Stir in citric acid to pH4 and 8% CaCl2 by weight. Heat gently to 150F. Cover pot with lid and keep it at this temperature using very low heat for at least eight hours.
  
 
== Pull ๐Ÿ‘ฉโ€๐Ÿ”ฌ==
 
== Pull ๐Ÿ‘ฉโ€๐Ÿ”ฌ==
โˆ’
Transfer treated liquid and bark to a mason quart jar (or a suitable container with a narrow lid). Add water if needed so quart jar is close to being full. Shake in ~65ml of light naphtha. Add lye and shake vigorously for a few minutes. Solution will warm up slightly as lye dissolves and will quickly go from red, to milky, to dark red.
+
Transfer treated liquid and bark to a mason quart jar (or another suitable container). Add water if needed so quart jar is close to being full. Shake in ~65ml of light naphtha. Add lye and shake vigorously for a few minutes. Solution will warm up slightly as lye dissolves and will quickly go from red, to milky, to dark red.
  
  
โˆ’
Rest solution until naphtha layer separates (~10 minutes, see Fig. 3). If separation is not complete after 30 minutes, mix in another 5g of lye and try again.
+
Rest jar in a warm water bath until naphtha layer separates (~10 minutes, see Fig. 3). If separation is not complete after 30 minutes, mix in another 5g of lye and try again.
  
  
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โˆ’
Add another ~65ml of naphtha to the quart jar. Shake for a few minutes, rest until layers separate, and pipette naphtha into the pint jar. Perform this step two more times (total of 4 pulls, including the first one).
+
Add another ~65ml of naphtha to the quart jar. Shake for a few minutes, rest in a warm water bath until layers separate, and pipette naphtha into the pint jar. Perform this step two more times (total of 4 pulls, including the first one).
  
  

Revision as of 00:21, 13 December 2021


Introduction ๐Ÿ™

Pure DMT free base can form white crystals, yellow powder, and orange to red wax/goo. This wide range of appearance could be due to self aggregation because of indole ring pi bond stacking [1] (see Fig. 1).


This technique (TEK) focuses on maximizing white crystalline DMT by minimizing self aggregation during extraction.


Thanks to benzyme for showing MS evidence of DMT weakly bonding to itself, and to Jees, downwardsfromzero, IridiumAndLace, and Loveall for their contributions to this process in the forum[2].


Dmt copy 800x364.png
Fig. 1: Mass spectrum of DMT goo (from benzyme). Peaks in multiples of 188m/z unmask the nature of DMT goo as DMT-DMT bonding aggregation (possibly through indole ring pi stacking).

Safety โ›‘๏ธ

Review NaOH[3] and naphtha [4] safety information. Verify solvent MSDS purity, plastic compatibility, and clean evaporation.


Never have solvents near an open flame.


Following this advice does not guarantee safety. It is up to each adult individual to make their own decision.

Materials๐Ÿ›’

Consumables๐Ÿ‘ฉโ€๐ŸŒพ

  • Water
  • 50g of mimosa hostilis root bark
  • 5g ascorbic acid
  • ~250ml of light hydrocarbonsโ€ 
  • 25g of NaOH


โ€ It is very important to use a source of light hydrocarbons. The smaller organic molecules seem to control DMT aggregation. Naptha used in paint applications tends to be too heavy. Petroleum distillate lighter fluids have molecules with smaller carbon chains and perform well (e.g. Ronsonol). Avoid products with anti rust or dies (e.g. Coleman camping fuel). Using the proper solvent is very important to control DMT aggregation if a white crystalline product is desired.

Equipment๐Ÿบ

  • Stovetop
  • Pot with lid
  • Quart and pint jars
  • Scale
  • Pipette
  • Freezer
  • Fan
  • Scraping tool

Process Overview ๐Ÿ‘€

  • Freeze/thaw bark 3x, treat with acid and CaCl2 150F for 8 hours, add light hydrocarbon solvent, basify gently with Ca(OH)2, pull/boil/evaporate/freeze solvent, decant/dry, scrape up.

Detailed Process ๐Ÿ“œ

Cell Lysing โ„๏ธ

Freeze/thaw bark mixed with 800ml of water in a pot with a lid. Repeat twice for a total of 3 times.


IMG 20211020 070456294 copy 800x801.jpg
Fig. 2: Pressure cooked bark in quart jars.

De-polymerization

Stir in citric acid to pH4 and 8% CaCl2 by weight. Heat gently to 150F. Cover pot with lid and keep it at this temperature using very low heat for at least eight hours.

Pull ๐Ÿ‘ฉโ€๐Ÿ”ฌ

Transfer treated liquid and bark to a mason quart jar (or another suitable container). Add water if needed so quart jar is close to being full. Shake in ~65ml of light naphtha. Add lye and shake vigorously for a few minutes. Solution will warm up slightly as lye dissolves and will quickly go from red, to milky, to dark red.


Rest jar in a warm water bath until naphtha layer separates (~10 minutes, see Fig. 3). If separation is not complete after 30 minutes, mix in another 5g of lye and try again.


Move naphtha into a pint jar with a pipette It is ok if a few drops of watery extract or bark particles come through (they will be decanted in the next section).


Add another ~65ml of naphtha to the quart jar. Shake for a few minutes, rest in a warm water bath until layers separate, and pipette naphtha into the pint jar. Perform this step two more times (total of 4 pulls, including the first one).


Ideally, all four pulls are done within an hour while the quart jar is slightly warm from the lye dissolving in water.


IMG 20211020 090639578 copy 600x1122 copy 427x800.jpg
Fig. 3: Settled naphtha pull ready to be pipetted.

Crystalize โœจ

Carefully decant naphtha pulls to a new fresh pint jar. Do not allow any watery extract or particles to come through.


Heat naptha in a water bath until so it boils (if it does not boil it is not light naphtha and could result in more goo). Boil for 10 minutes or until color stops changing to break up any DMT goo (red/orange colors indicative of goo will become more yellow).


Cool to room temperature and place naphtha in freezer to precipitate crystals*. Rest in freezer until cloudiness clears (at least 24 hours).


Decant naphtha off crystals, and immediately dry with the help of a fan. Once dry, dissolve xtals in a minimal amount of boiling fresh naphtha (~25ml) for 15 minutes, pout into a shallow baking dish, evaporate slowly (no fan), and scrape. This is the final product. Yields are typically 1 to 3%.


*If new naphtha was used, one option is to evaporate the solvent until slightly cloudy with the help of a fan in a well ventilated area. A better option is to skip the solvent evaporation. Yield will be lower by ~500mg if using new naphtha, but it will be available for reuse as a one-time "investment" for the next extraction. Subsequently, used naphtha does not need to be evaporated before freezing to get the full yield since it already comes preloaded with a DMT concentration that is saturated at the freezer temperature.

Reclaim Solvent ๐Ÿ’š

Reusing solvents is encouraged[5] at the DMT nexus.


Simply reuse freeze precipitated naphtha as-is. Re-used naphtha is saturated with DMT at freezer the temperature (~2mg/ml) and pre-freezer evaporation is not needed. Easy ๐Ÿ˜Š

Frequently Asked Questions โ“

Q: That's a lot of hypothesis you got down in the appendix. Have any experimental evidence consistent with them?

A: Yes. Benzyme's MS, together with polymerization and de-polymerization experiments. As far as we know experiments are consistent with the hypotheses listed. The community is welcome to update this Wiki entry as more evidence arises, especially if any of the hypotheses are disproved (thank you).


Q: What's so special about Vitamin C?

A: See the development notes in appendix below.


Q: Why are there only 3 pulls without a warm water bath or salting out ionic strength? Usually ~5 warm (40-50C) + high ionic strength pulls (~6% NaCl) are needed.

A: DMT monomer is highly soluble in naphtha and has an excellent partition coefficient. By converting natural DMT to this form, and keeping alkaline conditions gentle to avoid polymerization, the pulls are simpler and very efficient. No added heat or ionic strength is necessary.


Q: What is the difference between DMT polymers, oligomers, aggregates, and aromatic pi-pi stacking?

A: None, all names are equivalent and refer to the same thing: weakly bonded groups of DMT molecules that form goo instead of crystals.

Appendix: Development Notes ๐Ÿ”ฌ

Hypotheses ๐Ÿค”

This TEK hypothesizes that:


  • Not all of the DMT is in the plant in monomer form, some of it is in macro-molecule form (also called polymer, oligomer, or goo)
  • In addition to natural DMT polymer, even more polymer can form during the basing step under high alkaline, high ionic strength, and high DMT concentration conditions
  • Polymer can also form and be broken up I'm the solvent
  • Pressure cooker treatment of the bark, together with a separate warm vitamin C step is effective at breaking down any natural DMT polymer to the monomer form
  • Once natural DMT polymer is broken down, gentle alkaline conditions keep it from forming again
  • Goo can also form in the solvent. Slow evaporation of freeze precipitated product minimizes DMT-DMT bonding in the final product.
  • DMT monomer properties compared to DMT polymer:
    • Easier to dissolve in naphtha (better partition coefficient)
    • Barely clouds during naphtha evaporation
    • Slowly crashes during freeze precipitation as white crystals. In contrast, DMT polymer precipitates sooner as yellow/orange/red semisolid goo
    • Easier to handle and dose precisely
    • Low and consistent vaporization temperature, ideal for newer electronic vaporization devices with precisely tuned temperature settings
    • Visibly unique upon crystalization, eliminating questions around plant oil contaminants
    • May be easier to complex with HPBCD for sublingual administration
    • It is unknown if it has better bioavailability for oral or rectal administration. In principle, stomach acid should be able to break down DMT polymer, so perhaps there is no difference for oral administration
    • There is no expected benefit for torch vaporization by an experienced user since the strong heat produced manually can easily vaporize everything. However, the process window between vaporizing and burning the DMT is larger for the monomer which may benefit the inexperienced user

Strategy โ™Ÿ๏ธ

The strategy of this TEK is to break down both DMT aggregates and plant material, while minimizing DMT re-aggregation during the basing step.


Agressive alkaline concentration conditions are avoided. While these type of processes can break down plant material, their downside is that they don't break down natural DMT aggregates and can even increase the degree of polymerization.


Fortunately, DMT aggregates can break down in acidic conditions. Therefore, to simultaneously break down DMT aggregates and plant material, a long acidic pressure cooking step is used (described before by for example Northener). Vitamin C is used to complete de-aggregation due to its good experimental performance and some literature references referring to it's ability to disrupt pi-pi bonds[6], but other acids could also work. Subsequently, relatively gentle ionic strength (no added salt), gentle alkaline pH (no excess lye beyond emulsion breakdown), and low DMT concentration (<0.5%) conditions are used to minimize any DMT re-polymerization. Naphtha is introduced before basing to minimize the time bulk DMT spends in alkaline water.

Vitamin C ๐ŸŠ

Experimentally, Vitamin C produced better results compared to acetic and citric acids. Vitamin C is biologically active as a mild antioxidant and reducing agent and can pass through cell membranes.


Vitamin C begins to degrade at 158F. The activity of vitamin C decreases with temperature, so it is added when the extract is still hot yet below this degradation temperature.


A possible specific mechanism of action is that as a strong electron donor, vitamin C disrupts parallel displaced aromatic ring pi-bond stacking conformations[7][8].


Other acids may also work, and the kitchen alchemist is encouraged to report on any new experimental results (both positive and negative).

Cloudiness ๐ŸŒซ๏ธ

DMT monomer does not readily form clouds in naphtha compared to other extractions that do not minimize polymer. In this TEK clouds form later in the freezer or evaporation process and are not as opaque. Late cloud formation is a good sign and not a cause for concern. Monomer crystals take longer to grow in the freezer, so give them extra time.

References ๐Ÿ—๏ธ

  1. โ†‘ Polymer MS evidence[1]
  2. โ†‘ Minimum Polymer[2]
  3. โ†‘ NaOH safety[3]
  4. โ†‘ Naphtha safety[4]
  5. โ†‘ On reusing non polar solvent[5]
  6. โ†‘ Uric acid de-aggregation by vitamin C[6]
  7. โ†‘ Pi-bond aromatic stacking[7]
  8. โ†‘ Tryptophan parallel displaced stacking[8]