Edited by Mod to include the update presented on Page #2
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Update
Well, I figured it's about time to revamp this extraction overview. I'm adding a little bit more detail, and also adding in the FASA option.
I just wrote a brief chemistry lesson to explain the chemical principles behind the extraction. I've simplified the explanation so that a non-chemist can understand what's going on in the process. Understanfing the chemistry behind the process isn't critical to extracting, so I expect uninterested folks will skip over it, but it's a good crash-course in pratical chemistry to the interested layman. Also, I define several important chemical terms, so if someone doesn't understand what I'm talking about in the main Extraction Overview, they can glance back at the chemistry lesson portion for an explanation.
Once I finish the revision, I'll replace the first post in the thread with it. For now, I'll just leave it a work-in-progress in this post.
Answer to the Most Frequently Asked Question Regarding DMT Extractions: Which tek do I use?
I know there are plenty of people who don't want to read all this, and just want to know what's the simplest tek to use. I've seen this question posted a million times, so I figured I'd include my answer in here, so I can link to it easily.
For anyone who doesn't wish to weigh the merits of all the methods, here is my recommendation: As long as you're extracting from Mimosa hostilis root bark, use Noman's tek or Marsofold's tek. But, instead of the ammonia wash of the final product, use the sodium carbonate wash from Vovin's Tek (Step 7, pg 12). But be aware that a desire for simple answers may not serve you so well in your encounters with the spice.
How DMT Extractions work - The Chemical Principles
All DMT extraction teks are based on the relative solubilities of the DMT in it's protonated and unprotonated form. What does that mean exactly?
Lets start out with a crash-course some basic chemical principles. If you're familiar with acid/base equilibria and polar vs nonpolar solvents, feel free to skip ahead. If you don't want a chemistry lesson, likewise feel free to skip this section (though if you come across unfamiliar chemical terms in the extraction overview, check back here for definitions). All important terms are in bold so you can glance back and check the definition if you forget what it means.
Acids and Bases
A proton is a positively hydrogen ion, H+. The transfer of protons is the entire basis of acid/base chemistry. An acid is a molecule that can donate a proton. A base is a molecule that can acquire a proton.
Every acid has a conjugate base; for example, when acetic acid (CH3COOH) gives up the proton on its -COOH group (incidentally, this is called a "carboxylic acid"Pleased, its conjugate base is the acetate anion (CH3COO-). Thus acetic acid and acetate are called a "conjugate pair". Likewise, every base has a conjugate acid; for example, when ammonia (NH3) aquires a proton, its conjugate acid is an ammonium cation (NH4+). (Ammonia and ammonium are another conjugate pair).
Just a bit of terminology: An when a molecule carries a charge, we call it an ion. If it's positively charged, we call it a cation; if it's negatively charged, we call it an anion.
pH and pKa
The relative concentrations of each member of a conjugate pair in solution is determined by the pH. The lower the pH, the more protons there are in solution, and bases are eager to grab them up. The higher the pH, the less protons there are in solution, and the more eager the conjugate acids are to be rid of them. Low pH solutions are referred to as acidic, while high pH solutions are referred to as alkaline, or basic.
The pH where the concentrations of a base and its conjugate acid are equal is called the "pKa" of that conjugate pair. Above the pKa, more of the molecule exists in its base form; below the pKa, more of the molecule exists as its conjugate acid.
DMT is a neutral (uncharged) base, sometimes called a "freebase" because the uncharged ("free"Pleased base can be obtained as a solid. The pKa of DMT is 8.68. Above pH 8.68, it exists primarily in its neutral (uncharged) freebase form. Below pH 8.68, it exists primarily in its positively charged acid form.
[image]/forums/thumbs/08-45/574231359-thumb_DMT_baseacid.jpg[/image]
Salts
Often the protonated form of DMT will associate with a "counterion". When ions associate to form an complex with a net charge of 0, we call this a salt . Since DMT bears a positive charge, it must associate with a negatively charged ion in order to form a neutral salt. For example, if we acidify a solution of DMT using acetic acid, then the DMT will predominantly assume its charged (protonated) conjugate acid form, and will tend to associate with acetate ion (CH3COO-), the conjugate base of the acetic acid we used to acidify the solution. We would call the resulting salt DMT acetate.
So what does all this have to do with extracting DMT? Don't worry, we only need to talk about one more piece of the puzzle to start making sense of it.
Solvents
A solvent is a liquid in which other molecules can be dissolved. In the case of extractions, we're interested in dissolving DMT. For our purposes, there are two types of solvents: polar solvents, and nonpolar solvents. In polar solvents (like water and ethanol), polar compounds like salts and ions tend to be highly soluble (that is, they dissolve easily), while less polar compounds like hydrocarbons and neutral organic molecules (like DMT freebase) tend to be relatively insoluble (that is, they tend not to dissolve). In nonpolar solvents (like naphtha and dichloromethane) polar compounds tend to be insoluble, while less polar compounds tend to be more soluble. When polar and nonpolar solvents are mixed together, they typically stay seperated as two seperate layers, or "phases". Oil and water is the classic example of this phenomenon.
This is a simplified explanation, but it'll serve well enough to explain the basic principles of the process.
Now let's bring it all back home with respect to extracting DMT:
In acidic water, DMT exists predominantly in its protonated form, either as a cation or a salt. Since the protonated form of DMT is relatively polar, DMT is quite soluble in acidic water. In alkaline water, DMT exists predominantly in its freebase form. While the freebase is not particularly soluble in water, it's not so insoluble that it falls out of solution or forms a seperate layer. But if we were to mix an alkaline solution of DMT with a nonpolar solvent, since the DMT freebase is much more soluble in the nonpolar solvent, much of it will migrate from the polar solvent to the nonpolar solvent.
This is the basis of almost every DMT extraction.
That covers the theory side of things pretty well, now let's talk about the practical side of things.
How DMT Extractions Work - The Universal Procedure
All the teks around may look different on the surface, but they all boil down to three basic steps:
Step 1.) Make a solution of DMT
Step 2.) Extract the DMT into a nonpolar solvent
Step 3.) Recover the DMT from the nonpolar solvent as a solid
That's all there is too it. The rest is just details. And of course, we're also leaving out the preliminary step:
Step 0.) Selecting a plant to extract from
With these steps in mind, let's begin!
0 - Selecting a Plant to Extract From
The extractor has a fairly wide array of choices for their starting material (see the “DMT is Everywhere” chapter of TiHKAL), but the most popular choices are Mimosa and Acacia. If you are considering starting from some other material, you will want to think about the fat content of the material, and probably include more of the optional purification steps.
Mimosa hostilis root bark (MHRB) seems to be ideal; since it's low in plant fats, it's easy to achieve a pure product with minimal purification.
Acacia bark is also a good option, although you will want to be certain to have at least one acid-base process in your procedure, either as the initial extraction or a later purification. There are many species of Acacia that contain DMT (and many that do not). Extracting from Acacias is especially popular in Australia, where many Acacia species are native.
Other options include Chacruna (Psychotria viridis) and Chaliponga (Diplopterys cabrerana), though these tend to be less economical. Also, chaliponga contains both DMT and 5-MeO-DMT, so if you wanted just one or the other, you'd have to seperate them after extracting (this is not a difficult process).
Phalaris grass can be used, but it's rarely worth the effort. The potency varies drastically, but is almost always very low. That means processing a huge bulk of messy plant matter for a mediocre yield. What's more, some types of phalaris contain gramine, a toxic alkaloid that could potentially be extracted along with the DMT.
1 - Making a Solution of DMT
There are two main schools of thought on this step, exemplified by acid/base teks (like Marsofold's or Vovin's) on the one hand, and straight-to-base teks (like Noman's and Lazyman's) on the other.
In an acid/base (A/B) process, you extract the DMT from your plant matter into an acidic solution, then add a base (like NaOH) to this solution so that the DMT can be extracted into your nonpolar solvent. With a straight-to-base (STB) process, you skip the whole acidic extraction and just mix together water, NaOH, and plant material to make an alkaline mixture from which the DMT can be extracted into your nonpolar solvent.
There has recently emerged a third option (see the FASA Method) that forgoes the use of water, instead using acetone as the extraction solvent. At the time of this writing, there are no finished teks that utilize this procedure, but I wouldn't be surprised if it gains a lot of popularity in years to come, as it uses much safer materials than the currently popular extraction methods.
1.A - A/B: Extracting DMT Into An Acidic Solution
Simmer the plant material in water that has been acidified with your choice of acid to obtain a solution of the water soluble DMT salt. Hydrochloric, acetic, phosphoric, citric, and tartaric acids have all been used with good result.
It's important to simmer, not boil; the solution will lose potency if cooked at a full boil. The pH of the water is not particularly important. Older teks call for acidifying down to pH 1, but there's really no need to go lower than 4-5. Even neutral water that hasn't been acidified would still be relatively effective at extracting DMT; adding the acid just speeds up the process.
There is no clear answer to how many times one must cook the bark, or for how long, in order to extract most of the DMT. Generally, people use either two or three volumes of water, simmering each for anywhere between a half-hour and two hours.
There are two major advantages this method has over the straight-to-base teks. For one thing, it allows the extractor to use a seperatory funnel when extracting into their nonpolar solvent (Step 2). A seperatory funnel is the peice of glassware that chemists use when performing extractions, and it allows for easy seperation of the two solvent layers. The other advantage is that it allows the extractor to defat the extraction:
Optional: First Defatting Opportunity
You can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent. Many plant fats and other unwanted chemicals will migrate into the nonpolar phase, but the DMT will stay dissolved in the acidic water. The nonpolar solvent used for this step can then be discarded.
Naphtha, toluene, xylene, dichloromethane, and d-limonene are all acceptable nonpolar solvents for this step.
Defatting is not necessary for extracting from Mimosa hostilis rootbark, but it is important for virtually every other plant source of DMT.
1.B - STB: Making a Lye/Bark Stew
This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. In reality, it doesn't take much more time to do an A/B extraction compared with STB extractions, and they take about the same amount of actual effort. A disadvantage of this method is that it uses a lot more NaOH than A/B teks. Also it's not recommended if you're extracting from anything other than Mimosa, because it removes the opportunity to defat.
The basic idea is to simply cover the root bark with water basified to pH ~13 with NaOH and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of the NaOH is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Potassium hydroxide (KOH) could be used instead of sodium hydroxide (NaOH), but it's generally more expensive.
A good ratio of ingredients is 1 gram of NaOH and 15 mL of water for every gram of bark. If you use less water than this, the soup is too thick and some seriously nasty emulsions can form (see Step 2 for an explanation of emulsions). If you use less lye, yields go down (presumably because the bark is less thoroughly pulped) and emulsions are more likely to form (presumably because the excess NaOH increases the ionic strength of the soup; the higher the ionic strength is, the less naphtha likes getting trapped in there).
2 - Extract the DMT Into a Nonpolar Solvent
At this point, we want to extract DMT from an alkaline solution into a nonpolar solvent. The only major difference between A/B and STB teks at this step is that A/B extractors need to add a base (like NaOH) to make their solution alkaline, while an STB extractor's lye stew is already alkaline.
The basic idea is to mix an alkaline DMT solution with a nonpolar solvent. Since DMT will exist in its uncharged freebase form in alkaline solutions, and the freebase is much more soluble in nonpolar solvents than it is in water, much of the DMT will migrate into the nonpolar solvent when they're mixed.
Emulsions
When mixing together the alkaline DMT mixture and the nonpolar solvent, the extractor's biggest enemy is the dreaded emulsion. An emulsion is a suspension of bubbles of polar and nonpolar liquids trapped together. When you shake Italian dressing to mix together the oil and vinegar layers, your goal is to create an emulsion.
With a DMT extraction, you want to avoid emulsions as much as possible; they often take a very long time to seperate. Emulsions generally form when the nonpolar solvent and alkaline water are mixed too violently. Vigorously shaking your extraction, just like shaking a bottle of Italian dressing, will cause tiny droplets from both of the layers to get trapped in one another. When mixing the nonpolar solvent and the alkaline water, it's best to use a gentle swirling motion. Some people manually mix the layers with a spoon/utensil (before doing this, make sure that your mixing utensil is made of a material that will stand up to strong alkaline solutions and your nonpolar solvent; glass or HDPE#2 plastic is optimal). However you decide to mix the layers, don't shake them up too much.
People sometimes get confused about what an emulsion looks like. With a DMT extraction, it can look different depending on how severe the emulsion is. If you have a severe emulsion, the extraction will appear to only have a single layer; all of the nonpolar solvent is trapped in the akaline water layer. With a less severe emulsion, the extraction appears to have three layers: one is alkaline water, the other is nonpolar solvent, and in the middle between the other two there's a bubbly, soapy-looking layer (this middle layer is the emulsion).
Breaking An Emulsion
If you do end up with an emulsion, there are things you can do to seperate it (seperating an emulsion into seperate polar and nonpolar layers is known as "breaking" the emulsion).
Saturating the alkaline water with NaCl(table salt) can help to break the emulsion; the saltier the water is, the less happy the naphtha is being trapped in there. You'll probably want to buy the NaCl in the form of rock salt; granulated table salt has anti-caking chemicals and is sometimes iodized. In order to help prevent emulsions, some people choose to saturate their alkaline solution with NaCl before adding nonpolar solvent.
Heating up the extraction also encourages the layers to seperate - just be careful of the fumes from your nonpolar solvent.
If you're using an STB process, adding more water is sometimes crucial to breaking an emulsion. If you're extracting from Mimosa, sometimes more NaOH is required (Mimosa is more sensitive than other plants in this regard)
Nonpolar Solvent Choice
There are a lot of options when it comes to choosing your nonpolar solvent.
Naphtha is the most popular solvent. It doesn't pull DMT as efficiently as other solvents, but it's readily available in most countries. The biggest advantage of naphtha is that the solubility of DMT in naphtha is temperature-dependent. DMT is moderately soluble in room-temperature naphtha, but barely soluble in ice-cold naphtha. That means that the naphtha from an extraction can be put in the freezer, and clean DMT precipitates out, providing a pure product and allowing the naphtha to be reused (this is known as "freeze precipitation"Pleased.
Xylene and Toluene haven't traditionally been all that popular, but I wouldn't be surprised if their use becomes more widespread in the future. They have a few things to recommend them: Not only do they extract DMT more efficiently than naphtha, they also extract other psychoactive alkaloids (the so-called Jungle Spice alkaloids). In the past, the reason that they haven't been popular is that it takes such a damned long time to evaporate. Fortunately a new method (the FASA method) has been discovered that allows for easy precipitation of the alkaloids from xylene or toluene; they precipitate as the fumarate salt, but this can be readily freebased in a variety of ways.
Dichloromethane, or DCM, is about the most effective; it pulls the DMT well, and evaporates quickly (avoid inhaling the vapors!). Most people don't have access to dichloromethane, however. Diethyl ether is likewise effective, but its combustablility makes it more dangerous for the inexperienced handler.
2.A - A/B: Freebasing and Extracting
Before extracting, you need to add a base to raise the pH of the water. Depending on how you're extracting, you have different choices of which base to use.
If you're extracting from something other than Mimosa hostilis, then you have several options. You basically just need to get the pH up to about 10. This can be accomplished most easily with sodium carbonate, though of course stronger bases may be used.
If you're extracting from Mimosa rootbark, then pH 10 is no good; when the pH of the aqueous Mimosa extract is in the 95.-12.5 range, it turns a thick gritty gray color. If you try to extract from it, you're apt to get an awful emulsion. Once the pH is raised to about 13, the color changes again to a slippery black/brown color, and emulsions won't form unless you really over-agitate the mixture. Because you need to get the pH so high, NaOH (lye) or KOH are about your only options. Calcium hydroxide could also be used, though it's a bit messier dealing with insoluble calcium salts. The only exception to this is if you're extracting with DCM; apparently DCM won't form emulsions even at pH 10, so you can basify with sodium carbonate (washing soda, notbaking soda) if you want to avoid using lye.
Once you've basified your acidic extract, you're ready to add your nonpolar solvent and begin extracting.
2.B - STB: Extracting from Lye-Bark Stew
With an STB extraction, your aqueous mixture is already alkaline, so you're ready to just add your non-polar solvent and begin extracting.
When going this route, a basic polar wash (like a sodium carbonate wash) on your nonpolar solvent is practically a must; without it, the product is typically harsher to smoke.
Optional: Polar Wash of Nonpolar Solvent
This can be done whether you're doing an A/B or STB extraction. It's probably not important for A/B extractions, but it is recommended with STBs.
The idea here is to remove any lye (or other base) that may have made it into your nonpolar solvent. Although NaOH is completely insoluble in naphtha, it's still possible for it to enter the naphtha phase as a kind of microparticulate dust.
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Original Post
The following is not a Tek, but rather a concordance of Teks. Virtually all DMT extractions follow the same basic process; they differ only in whether the initial extract is acidified, and in what purification techniques they prefer. I posted it on another forum (the Shroomery), but figured it might be of use to some folks here.
The internet community has really stepped up in terms of providing step-by-step walkthroughs to guide the layman through the process of extracting DMT crystals. A quick search for DMT extraction teks turns up dozens of procedures; but how’s a body to know which tek to choose? I've seen a lot of posts by people having problems with purity due to trying to follow a tek too closely (especially ones that don't give the reader a target pH).
Really though, all of the teks out there boil down to the same process: Extract DMT into an aqueous solution, collect DMT as the freebase in a nonpolar solvent, then recover the freebase as a solid. All of the differences between teks are just differences in purification techniques. And depending on your starting material and available chemicals, the purification steps in any given tek may not suit your extraction. Which is why I've written the following extraction overview, so the extractor can chart a plan of attack that best suits their extracting conditions. I'm not going to go into mundane detail on accomplishing any particular step, just give enough information that someone acquainted with basic extraction processes could easily accomplish it. This level of detail is covered thoroughly in the teks.
Answer to the Most Frequently Asked Question Regarding DMT Extractions: Which tek do I use?
I know there are plenty of people who don't want to read all this, and just want to know what's the simplest tek to use. I've seen this question posted a million times, so I figured I'd include my answer in here, so I can link to it easily.
For anyone who doesn't wish to weigh the merits of all the methods, here is my recommendation: As long as you're extracting from Mimosa hostilis root bark, use Noman's tek or Marsofold's tek. But, instead of the ammonia wash of the final product, use the sodium carbonate wash from Vovin's Tek (Step 7, pg 12). But be aware that a desire for simple answers may not serve you so well in your encounters with the spice.
1. Extraction of the Plant Material
Obviously the extractor has a fairly wide array of choices for a starting material to extract from (see the “DMT is Everywhere” chapter of TiHKAL), but the most popular choices are Mimosa and Acacia. If you are considering starting from some other material, you will want to think about the fat content of the material, and probably include more of the optional purification steps. Mimosa seems to be ideal, since many people report surprisingly pure product with minimal purification. Acacia is also a good option, although you will want to be certain to have at least one acid-base process in your procedure, either as the initial extraction or a later purification.
When it comes to the actual extraction from the plant material, there are essentially only two general processes to choose from:
• Acid/Base Extraction – Heat the plant material in water that has been acidified to pH 2-4 with your choice of acid to obtain a solution of the water soluble DMT salt. Hydrochloric, acetic, phosphoric, citric, and tartaric acids have all been used with good result. If you’re using any plant material other than Mimosa, it’s recommended that you follow this route because it lends itself to more thorough purification of the product.
• Straight to Base Extraction – This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. The basic idea is to simply cover the root bark with water basified to pH ~13 and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of hydroxide is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Sodium hydroxide is by far the most popular choice, though potassium hydroxide could be used instead. When going this route, a basic polar wash on your nonpolar solvent is practically a must; otherwise, some residual lye seems to remain in the product, making it more harsh. In the US, NaOH is a watched chemical due to its use in meth production. Ordering online or buying with a credit card could have undesired concsequences.
(Optional) First Defatting Opportunity (Acid/Base Extraction Only)
If you made an acidic extract of the DMT salt, you can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent and the solvent discarded. Naphtha, toluene, or xylene are all acceptable for this step.
2. Nonpolar Extraction of the Freebase
At this point it’s time to recover your DMT freebase into a nonpolar solvent. Xylene and toluene are not recommended for this step, particularly with Mimosa, as they will carry along a red pigment that can end up in your final product (some people extract with these solvents with the explicit intent of extracting the red pigment, which has been reported to be psychoactive itself). Naphtha is the most commonly used solvent for this step, but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well. Remember when extracting, you want to swirl or gently mix the layers, not shake them. Nasty emulsions can form, which are to be avoided at all costs.
• Acid/Base Extractors – Now you need to deprotonate your DMT back to the freebase. This is done by adjusting your acidic extract to pH > ~9.5 . Typically this is done by adding sodium hydroxide depending on what pH you're aiming for. If necessary, the volume of the acidic solution may be reduced before basifying. The basic solution is then extracted with several volumes of nonpolar solvent. These extractions may be pooled unless you want to process them individually. The basic solution now theoretically been stripped of DMT, and can be discarded. There is some debate over the optimal pH for this step. It's known that with certain plants sources (like Chacruna), a pH of 9 is sufficient to achieve maximum yields. On the other hand, Mimosa extractors have found that a much higher pH is necessary; this is likely due to the effects of various phytochemical solutes on the polarity of the aqueous phase. In theory, the addition of excess salt to the aqueous phase of a Mimosa extract prior to defatting ought to accomplish the same thing as the tremendous excess of hydroxide, but I've not yet heard of this being successful.
• Straight to Base Extractors – Your solution is already basic, so you’re good to go on this step. Just extract your basic, bark-filled mixture with several volumes of nonpolar solvent. The volumes may be pooled or processed individually.
(Optional) Acid/Base Purification and Defatting
If you did an acid/base extraction, this step is probably unnecessary, especially if you defatted before recovering the freebase. It can be done if you’re really worried about impurities and aren’t partial to any of the subsequent purification methods. If you went straight to base, then this step could be worth your while, as it allows you to defat your extract. On the other hand, many people find that Mimosa has little enough fat content that defatting leads to an unnecessary loss of product.
Extract your nonpolar DMT freebase solution with several volumes of water acidified to pH 3-4 with your choice of acid (hydrochloric, acetic, tartaric, etc.) and pool the extracts. If desired, defat the acidic solution with a couple volumes of nonpolar solvent (naphtha, toluene, etc.). Basify the solution to regenerate DMT freebase and recover by extracting with several volumes of extracting solvent (naphtha, DCM, hexanes, etc.), pooling the extracts.
(Optional) Washing the Nonpolar Solution
Many teks don’t include this process, which comes from Vovin's Tek, but it seems to be the best option for those concerned about residual lye in the nonpolar phase. To neutralize any lye which still remains in your product, wash the nonpolar solution of freebase with a small volume of dilute sodium carbonate (washing soda), pH ~8.5 (this is not the same as baking soda, sodium bicarbonate). The layers separate easily without emulsion, so shake away, then drain the water from the bottom of your seperatory funnel (assuming you’re using naphtha so your organic layer is on top). Room temperature water should be used for the sodium carbonate solution to avoid cooling the naphtha and encouraging precipitation. If desired, you can perform a couple more quick washes with neutral (unbasified) water to remove any traces of the sodium carbonate which may have been left in the naphtha.
3. Recovering the DMT Freebase from Solvent
There are basically two schools of thought on this step: evaporate the solvent or precipitate DMT crystals by freezing. There’s nothing really wrong with simply evaporating if you’re going to be doing further purification on the material, but that being said, I still don’t really see any reason to do it until you’ve freeze-precipitated a majority of your product.
To freeze precipitate, separate the nonpolar solvent from the aqueous phase and place the nonpolar solvent in the freezer (with the temperature setting as cold as it will go), and allow it to sit overnight. Depending on how concentrated the solution is, a good portion of DMT ought to precipitate out as nice crystals. These crystals can be removed but must be dried quickly or in a cold environment, because they will redissolve as the solvent warms up. At this point your best bet is probably to reduce the nonpolar solution to something less than half its original volume, and freeze precipitate again. Repeat until no crystals result or the crystals have significant visible impurities, at which point you can either discard the remaining mess, or evaporate the nonpolar solvent and recover the last shreds of DMT by further purification. In a simple variation on freeze precipitation, some people report success in growing larger crystals by repeatedly transferring the recrystallizing solution back and forth between the freezer and fridge every few hours.
Now the only thing left to do is purify the loot.
(Optional) Wash Crystals with Cold Aqueous Ammonia (Not Recommended!!!)
This is a simple way to wash out some minor impurities and discoloration. Just set up a filtration apparatus, put the crude DMT on the filter, and rinse with a small volume of ice-cold aqueous ammonia (preferably 10% concentration). Many people have run into problem with this method, resulting in the ammonia dissolving away their product, making it difficult to recover.
(Optional) Recrystallize from Hot Solvent
This will help to reduce impurities and give the product a more sharply defined melting point, but it won’t do much to reduce discoloration unless combined with activated charcoal (see below). To recrystallize, dissolve your product in a minimal volume of hot solvent (e.g. roughly 20 mL naphtha per gram of DMT). This will probably leave an undissolved sludge at the bottom of the vessel; the DMT-laden solvent can generally be separated from the sludge by simple decanting. Allow the solution to cool slowly with minimal agitation. Once it has reached room temperature, transfer it to the fridge for a couple hours, then to the freezer. Though it’s not necessary, if you have a small DMT crystal on hand, you can add it to the solution to help seed the recrystallization. Regardless, a nice crop of crystals should precipitate out of solution, and can now be collected by filtration. If unsatisfied with the results of a recrystallization, you can always reheat the solvent to redissolve the DMT and reduce the solution volume, then repeat the cooling process. Naphtha is the most commonly used recrystallization solvent, but success has also been reported with hexane.
(Optional) Clean with Activated Charcoal
This seems to be the most effective and reliable method for removing discoloration. Proceed exactly as though you were recrystallizing, but after dissolving the DMT in hot solvent, add a small quantity of crushed activated charcoal and swirl occasionally, sustaining heat for about ten minutes. Decant the hot solvent from the charcoal and allow to crystallize as usual. This method generally removes only discoloration-related impurities and requires a fairly clean starting, which is why I don’t recommend doing it with the crude nonpolar freebase solution prior to the initial freeze-precipitation.
(Optional) Acid/Base Purification and Defatting
Unless your extraction was extremely messy and gave you a gunky mess instead of crystals, then this step is total overkill. If your product is a roughly crystalline solid, a wash with cold aqueous ammonia and recrystallization with activated charcoal treatment should clean it up just fine. But if you want to recover any DMT from the gunk you get evaporating your solvent after freeze-precipitating, this is the way to do it. Take up the crude material in water adjust to pH 3-4 with your choice of acid. Defat if desired, then basify, extract, and precipitate.
(Optional) Purify by Column Chromatography
Obviously this route is not for the average extractor, and assumes you have access to a chromatography column, or at least a buret which can function the same on a smaller scale. It is totally unnecessary unless you're aiming for analytic purity or you have a godawful extraction goo that calls for some heavy-duty purification. You may run a TLC first using the same solvent pair that you plan to run the column with to get an idea what you'll be up against, but this is probably not necessary. The DMT can be visiualized under UV light as a blue spot.
Plug the stopcock end of your buret or column with a glass wool (or less ideally, cotton) filter. Cover this with a small portion of sand and fill your column with silica slurry. Load your crude sample, and elute with your chosen solvent pair. Monitor the progress of the DMT with a UV light to capture the correct fraction. If you don't understand what any of this means, you probably shouldn't attempt it, but you can consult a lab manual to satisfy your curiosity.
Well, there you have it. If anyone knows of any other common or effective purification techniques, I'd be interested.
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Update
Well, I figured it's about time to revamp this extraction overview. I'm adding a little bit more detail, and also adding in the FASA option.
I just wrote a brief chemistry lesson to explain the chemical principles behind the extraction. I've simplified the explanation so that a non-chemist can understand what's going on in the process. Understanfing the chemistry behind the process isn't critical to extracting, so I expect uninterested folks will skip over it, but it's a good crash-course in pratical chemistry to the interested layman. Also, I define several important chemical terms, so if someone doesn't understand what I'm talking about in the main Extraction Overview, they can glance back at the chemistry lesson portion for an explanation.
Once I finish the revision, I'll replace the first post in the thread with it. For now, I'll just leave it a work-in-progress in this post.
Answer to the Most Frequently Asked Question Regarding DMT Extractions: Which tek do I use?
I know there are plenty of people who don't want to read all this, and just want to know what's the simplest tek to use. I've seen this question posted a million times, so I figured I'd include my answer in here, so I can link to it easily.
For anyone who doesn't wish to weigh the merits of all the methods, here is my recommendation: As long as you're extracting from Mimosa hostilis root bark, use Noman's tek or Marsofold's tek. But, instead of the ammonia wash of the final product, use the sodium carbonate wash from Vovin's Tek (Step 7, pg 12). But be aware that a desire for simple answers may not serve you so well in your encounters with the spice.
How DMT Extractions work - The Chemical Principles
All DMT extraction teks are based on the relative solubilities of the DMT in it's protonated and unprotonated form. What does that mean exactly?
Lets start out with a crash-course some basic chemical principles. If you're familiar with acid/base equilibria and polar vs nonpolar solvents, feel free to skip ahead. If you don't want a chemistry lesson, likewise feel free to skip this section (though if you come across unfamiliar chemical terms in the extraction overview, check back here for definitions). All important terms are in bold so you can glance back and check the definition if you forget what it means.
Acids and Bases
A proton is a positively hydrogen ion, H+. The transfer of protons is the entire basis of acid/base chemistry. An acid is a molecule that can donate a proton. A base is a molecule that can acquire a proton.
Every acid has a conjugate base; for example, when acetic acid (CH3COOH) gives up the proton on its -COOH group (incidentally, this is called a "carboxylic acid"Pleased, its conjugate base is the acetate anion (CH3COO-). Thus acetic acid and acetate are called a "conjugate pair". Likewise, every base has a conjugate acid; for example, when ammonia (NH3) aquires a proton, its conjugate acid is an ammonium cation (NH4+). (Ammonia and ammonium are another conjugate pair).
Just a bit of terminology: An when a molecule carries a charge, we call it an ion. If it's positively charged, we call it a cation; if it's negatively charged, we call it an anion.
pH and pKa
The relative concentrations of each member of a conjugate pair in solution is determined by the pH. The lower the pH, the more protons there are in solution, and bases are eager to grab them up. The higher the pH, the less protons there are in solution, and the more eager the conjugate acids are to be rid of them. Low pH solutions are referred to as acidic, while high pH solutions are referred to as alkaline, or basic.
The pH where the concentrations of a base and its conjugate acid are equal is called the "pKa" of that conjugate pair. Above the pKa, more of the molecule exists in its base form; below the pKa, more of the molecule exists as its conjugate acid.
DMT is a neutral (uncharged) base, sometimes called a "freebase" because the uncharged ("free"Pleased base can be obtained as a solid. The pKa of DMT is 8.68. Above pH 8.68, it exists primarily in its neutral (uncharged) freebase form. Below pH 8.68, it exists primarily in its positively charged acid form.
[image]/forums/thumbs/08-45/574231359-thumb_DMT_baseacid.jpg[/image]
Salts
Often the protonated form of DMT will associate with a "counterion". When ions associate to form an complex with a net charge of 0, we call this a salt . Since DMT bears a positive charge, it must associate with a negatively charged ion in order to form a neutral salt. For example, if we acidify a solution of DMT using acetic acid, then the DMT will predominantly assume its charged (protonated) conjugate acid form, and will tend to associate with acetate ion (CH3COO-), the conjugate base of the acetic acid we used to acidify the solution. We would call the resulting salt DMT acetate.
So what does all this have to do with extracting DMT? Don't worry, we only need to talk about one more piece of the puzzle to start making sense of it.
Solvents
A solvent is a liquid in which other molecules can be dissolved. In the case of extractions, we're interested in dissolving DMT. For our purposes, there are two types of solvents: polar solvents, and nonpolar solvents. In polar solvents (like water and ethanol), polar compounds like salts and ions tend to be highly soluble (that is, they dissolve easily), while less polar compounds like hydrocarbons and neutral organic molecules (like DMT freebase) tend to be relatively insoluble (that is, they tend not to dissolve). In nonpolar solvents (like naphtha and dichloromethane) polar compounds tend to be insoluble, while less polar compounds tend to be more soluble. When polar and nonpolar solvents are mixed together, they typically stay seperated as two seperate layers, or "phases". Oil and water is the classic example of this phenomenon.
This is a simplified explanation, but it'll serve well enough to explain the basic principles of the process.
Now let's bring it all back home with respect to extracting DMT:
In acidic water, DMT exists predominantly in its protonated form, either as a cation or a salt. Since the protonated form of DMT is relatively polar, DMT is quite soluble in acidic water. In alkaline water, DMT exists predominantly in its freebase form. While the freebase is not particularly soluble in water, it's not so insoluble that it falls out of solution or forms a seperate layer. But if we were to mix an alkaline solution of DMT with a nonpolar solvent, since the DMT freebase is much more soluble in the nonpolar solvent, much of it will migrate from the polar solvent to the nonpolar solvent.
This is the basis of almost every DMT extraction.
That covers the theory side of things pretty well, now let's talk about the practical side of things.
How DMT Extractions Work - The Universal Procedure
All the teks around may look different on the surface, but they all boil down to three basic steps:
Step 1.) Make a solution of DMT
Step 2.) Extract the DMT into a nonpolar solvent
Step 3.) Recover the DMT from the nonpolar solvent as a solid
That's all there is too it. The rest is just details. And of course, we're also leaving out the preliminary step:
Step 0.) Selecting a plant to extract from
With these steps in mind, let's begin!
0 - Selecting a Plant to Extract From
The extractor has a fairly wide array of choices for their starting material (see the “DMT is Everywhere” chapter of TiHKAL), but the most popular choices are Mimosa and Acacia. If you are considering starting from some other material, you will want to think about the fat content of the material, and probably include more of the optional purification steps.
Mimosa hostilis root bark (MHRB) seems to be ideal; since it's low in plant fats, it's easy to achieve a pure product with minimal purification.
Acacia bark is also a good option, although you will want to be certain to have at least one acid-base process in your procedure, either as the initial extraction or a later purification. There are many species of Acacia that contain DMT (and many that do not). Extracting from Acacias is especially popular in Australia, where many Acacia species are native.
Other options include Chacruna (Psychotria viridis) and Chaliponga (Diplopterys cabrerana), though these tend to be less economical. Also, chaliponga contains both DMT and 5-MeO-DMT, so if you wanted just one or the other, you'd have to seperate them after extracting (this is not a difficult process).
Phalaris grass can be used, but it's rarely worth the effort. The potency varies drastically, but is almost always very low. That means processing a huge bulk of messy plant matter for a mediocre yield. What's more, some types of phalaris contain gramine, a toxic alkaloid that could potentially be extracted along with the DMT.
1 - Making a Solution of DMT
There are two main schools of thought on this step, exemplified by acid/base teks (like Marsofold's or Vovin's) on the one hand, and straight-to-base teks (like Noman's and Lazyman's) on the other.
In an acid/base (A/B) process, you extract the DMT from your plant matter into an acidic solution, then add a base (like NaOH) to this solution so that the DMT can be extracted into your nonpolar solvent. With a straight-to-base (STB) process, you skip the whole acidic extraction and just mix together water, NaOH, and plant material to make an alkaline mixture from which the DMT can be extracted into your nonpolar solvent.
There has recently emerged a third option (see the FASA Method) that forgoes the use of water, instead using acetone as the extraction solvent. At the time of this writing, there are no finished teks that utilize this procedure, but I wouldn't be surprised if it gains a lot of popularity in years to come, as it uses much safer materials than the currently popular extraction methods.
1.A - A/B: Extracting DMT Into An Acidic Solution
Simmer the plant material in water that has been acidified with your choice of acid to obtain a solution of the water soluble DMT salt. Hydrochloric, acetic, phosphoric, citric, and tartaric acids have all been used with good result.
It's important to simmer, not boil; the solution will lose potency if cooked at a full boil. The pH of the water is not particularly important. Older teks call for acidifying down to pH 1, but there's really no need to go lower than 4-5. Even neutral water that hasn't been acidified would still be relatively effective at extracting DMT; adding the acid just speeds up the process.
There is no clear answer to how many times one must cook the bark, or for how long, in order to extract most of the DMT. Generally, people use either two or three volumes of water, simmering each for anywhere between a half-hour and two hours.
There are two major advantages this method has over the straight-to-base teks. For one thing, it allows the extractor to use a seperatory funnel when extracting into their nonpolar solvent (Step 2). A seperatory funnel is the peice of glassware that chemists use when performing extractions, and it allows for easy seperation of the two solvent layers. The other advantage is that it allows the extractor to defat the extraction:
Optional: First Defatting Opportunity
You can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent. Many plant fats and other unwanted chemicals will migrate into the nonpolar phase, but the DMT will stay dissolved in the acidic water. The nonpolar solvent used for this step can then be discarded.
Naphtha, toluene, xylene, dichloromethane, and d-limonene are all acceptable nonpolar solvents for this step.
Defatting is not necessary for extracting from Mimosa hostilis rootbark, but it is important for virtually every other plant source of DMT.
1.B - STB: Making a Lye/Bark Stew
This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. In reality, it doesn't take much more time to do an A/B extraction compared with STB extractions, and they take about the same amount of actual effort. A disadvantage of this method is that it uses a lot more NaOH than A/B teks. Also it's not recommended if you're extracting from anything other than Mimosa, because it removes the opportunity to defat.
The basic idea is to simply cover the root bark with water basified to pH ~13 with NaOH and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of the NaOH is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Potassium hydroxide (KOH) could be used instead of sodium hydroxide (NaOH), but it's generally more expensive.
A good ratio of ingredients is 1 gram of NaOH and 15 mL of water for every gram of bark. If you use less water than this, the soup is too thick and some seriously nasty emulsions can form (see Step 2 for an explanation of emulsions). If you use less lye, yields go down (presumably because the bark is less thoroughly pulped) and emulsions are more likely to form (presumably because the excess NaOH increases the ionic strength of the soup; the higher the ionic strength is, the less naphtha likes getting trapped in there).
2 - Extract the DMT Into a Nonpolar Solvent
At this point, we want to extract DMT from an alkaline solution into a nonpolar solvent. The only major difference between A/B and STB teks at this step is that A/B extractors need to add a base (like NaOH) to make their solution alkaline, while an STB extractor's lye stew is already alkaline.
The basic idea is to mix an alkaline DMT solution with a nonpolar solvent. Since DMT will exist in its uncharged freebase form in alkaline solutions, and the freebase is much more soluble in nonpolar solvents than it is in water, much of the DMT will migrate into the nonpolar solvent when they're mixed.
Emulsions
When mixing together the alkaline DMT mixture and the nonpolar solvent, the extractor's biggest enemy is the dreaded emulsion. An emulsion is a suspension of bubbles of polar and nonpolar liquids trapped together. When you shake Italian dressing to mix together the oil and vinegar layers, your goal is to create an emulsion.
With a DMT extraction, you want to avoid emulsions as much as possible; they often take a very long time to seperate. Emulsions generally form when the nonpolar solvent and alkaline water are mixed too violently. Vigorously shaking your extraction, just like shaking a bottle of Italian dressing, will cause tiny droplets from both of the layers to get trapped in one another. When mixing the nonpolar solvent and the alkaline water, it's best to use a gentle swirling motion. Some people manually mix the layers with a spoon/utensil (before doing this, make sure that your mixing utensil is made of a material that will stand up to strong alkaline solutions and your nonpolar solvent; glass or HDPE#2 plastic is optimal). However you decide to mix the layers, don't shake them up too much.
People sometimes get confused about what an emulsion looks like. With a DMT extraction, it can look different depending on how severe the emulsion is. If you have a severe emulsion, the extraction will appear to only have a single layer; all of the nonpolar solvent is trapped in the akaline water layer. With a less severe emulsion, the extraction appears to have three layers: one is alkaline water, the other is nonpolar solvent, and in the middle between the other two there's a bubbly, soapy-looking layer (this middle layer is the emulsion).
Breaking An Emulsion
If you do end up with an emulsion, there are things you can do to seperate it (seperating an emulsion into seperate polar and nonpolar layers is known as "breaking" the emulsion).
Saturating the alkaline water with NaCl(table salt) can help to break the emulsion; the saltier the water is, the less happy the naphtha is being trapped in there. You'll probably want to buy the NaCl in the form of rock salt; granulated table salt has anti-caking chemicals and is sometimes iodized. In order to help prevent emulsions, some people choose to saturate their alkaline solution with NaCl before adding nonpolar solvent.
Heating up the extraction also encourages the layers to seperate - just be careful of the fumes from your nonpolar solvent.
If you're using an STB process, adding more water is sometimes crucial to breaking an emulsion. If you're extracting from Mimosa, sometimes more NaOH is required (Mimosa is more sensitive than other plants in this regard)
Nonpolar Solvent Choice
There are a lot of options when it comes to choosing your nonpolar solvent.
Naphtha is the most popular solvent. It doesn't pull DMT as efficiently as other solvents, but it's readily available in most countries. The biggest advantage of naphtha is that the solubility of DMT in naphtha is temperature-dependent. DMT is moderately soluble in room-temperature naphtha, but barely soluble in ice-cold naphtha. That means that the naphtha from an extraction can be put in the freezer, and clean DMT precipitates out, providing a pure product and allowing the naphtha to be reused (this is known as "freeze precipitation"Pleased.
Xylene and Toluene haven't traditionally been all that popular, but I wouldn't be surprised if their use becomes more widespread in the future. They have a few things to recommend them: Not only do they extract DMT more efficiently than naphtha, they also extract other psychoactive alkaloids (the so-called Jungle Spice alkaloids). In the past, the reason that they haven't been popular is that it takes such a damned long time to evaporate. Fortunately a new method (the FASA method) has been discovered that allows for easy precipitation of the alkaloids from xylene or toluene; they precipitate as the fumarate salt, but this can be readily freebased in a variety of ways.
Dichloromethane, or DCM, is about the most effective; it pulls the DMT well, and evaporates quickly (avoid inhaling the vapors!). Most people don't have access to dichloromethane, however. Diethyl ether is likewise effective, but its combustablility makes it more dangerous for the inexperienced handler.
2.A - A/B: Freebasing and Extracting
Before extracting, you need to add a base to raise the pH of the water. Depending on how you're extracting, you have different choices of which base to use.
If you're extracting from something other than Mimosa hostilis, then you have several options. You basically just need to get the pH up to about 10. This can be accomplished most easily with sodium carbonate, though of course stronger bases may be used.
If you're extracting from Mimosa rootbark, then pH 10 is no good; when the pH of the aqueous Mimosa extract is in the 95.-12.5 range, it turns a thick gritty gray color. If you try to extract from it, you're apt to get an awful emulsion. Once the pH is raised to about 13, the color changes again to a slippery black/brown color, and emulsions won't form unless you really over-agitate the mixture. Because you need to get the pH so high, NaOH (lye) or KOH are about your only options. Calcium hydroxide could also be used, though it's a bit messier dealing with insoluble calcium salts. The only exception to this is if you're extracting with DCM; apparently DCM won't form emulsions even at pH 10, so you can basify with sodium carbonate (washing soda, notbaking soda) if you want to avoid using lye.
Once you've basified your acidic extract, you're ready to add your nonpolar solvent and begin extracting.
2.B - STB: Extracting from Lye-Bark Stew
With an STB extraction, your aqueous mixture is already alkaline, so you're ready to just add your non-polar solvent and begin extracting.
When going this route, a basic polar wash (like a sodium carbonate wash) on your nonpolar solvent is practically a must; without it, the product is typically harsher to smoke.
Optional: Polar Wash of Nonpolar Solvent
This can be done whether you're doing an A/B or STB extraction. It's probably not important for A/B extractions, but it is recommended with STBs.
The idea here is to remove any lye (or other base) that may have made it into your nonpolar solvent. Although NaOH is completely insoluble in naphtha, it's still possible for it to enter the naphtha phase as a kind of microparticulate dust.
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Original Post
The following is not a Tek, but rather a concordance of Teks. Virtually all DMT extractions follow the same basic process; they differ only in whether the initial extract is acidified, and in what purification techniques they prefer. I posted it on another forum (the Shroomery), but figured it might be of use to some folks here.
The internet community has really stepped up in terms of providing step-by-step walkthroughs to guide the layman through the process of extracting DMT crystals. A quick search for DMT extraction teks turns up dozens of procedures; but how’s a body to know which tek to choose? I've seen a lot of posts by people having problems with purity due to trying to follow a tek too closely (especially ones that don't give the reader a target pH).
Really though, all of the teks out there boil down to the same process: Extract DMT into an aqueous solution, collect DMT as the freebase in a nonpolar solvent, then recover the freebase as a solid. All of the differences between teks are just differences in purification techniques. And depending on your starting material and available chemicals, the purification steps in any given tek may not suit your extraction. Which is why I've written the following extraction overview, so the extractor can chart a plan of attack that best suits their extracting conditions. I'm not going to go into mundane detail on accomplishing any particular step, just give enough information that someone acquainted with basic extraction processes could easily accomplish it. This level of detail is covered thoroughly in the teks.
Answer to the Most Frequently Asked Question Regarding DMT Extractions: Which tek do I use?
I know there are plenty of people who don't want to read all this, and just want to know what's the simplest tek to use. I've seen this question posted a million times, so I figured I'd include my answer in here, so I can link to it easily.
For anyone who doesn't wish to weigh the merits of all the methods, here is my recommendation: As long as you're extracting from Mimosa hostilis root bark, use Noman's tek or Marsofold's tek. But, instead of the ammonia wash of the final product, use the sodium carbonate wash from Vovin's Tek (Step 7, pg 12). But be aware that a desire for simple answers may not serve you so well in your encounters with the spice.
1. Extraction of the Plant Material
Obviously the extractor has a fairly wide array of choices for a starting material to extract from (see the “DMT is Everywhere” chapter of TiHKAL), but the most popular choices are Mimosa and Acacia. If you are considering starting from some other material, you will want to think about the fat content of the material, and probably include more of the optional purification steps. Mimosa seems to be ideal, since many people report surprisingly pure product with minimal purification. Acacia is also a good option, although you will want to be certain to have at least one acid-base process in your procedure, either as the initial extraction or a later purification.
When it comes to the actual extraction from the plant material, there are essentially only two general processes to choose from:
• Acid/Base Extraction – Heat the plant material in water that has been acidified to pH 2-4 with your choice of acid to obtain a solution of the water soluble DMT salt. Hydrochloric, acetic, phosphoric, citric, and tartaric acids have all been used with good result. If you’re using any plant material other than Mimosa, it’s recommended that you follow this route because it lends itself to more thorough purification of the product.
• Straight to Base Extraction – This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. The basic idea is to simply cover the root bark with water basified to pH ~13 and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of hydroxide is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Sodium hydroxide is by far the most popular choice, though potassium hydroxide could be used instead. When going this route, a basic polar wash on your nonpolar solvent is practically a must; otherwise, some residual lye seems to remain in the product, making it more harsh. In the US, NaOH is a watched chemical due to its use in meth production. Ordering online or buying with a credit card could have undesired concsequences.
(Optional) First Defatting Opportunity (Acid/Base Extraction Only)
If you made an acidic extract of the DMT salt, you can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent and the solvent discarded. Naphtha, toluene, or xylene are all acceptable for this step.
2. Nonpolar Extraction of the Freebase
At this point it’s time to recover your DMT freebase into a nonpolar solvent. Xylene and toluene are not recommended for this step, particularly with Mimosa, as they will carry along a red pigment that can end up in your final product (some people extract with these solvents with the explicit intent of extracting the red pigment, which has been reported to be psychoactive itself). Naphtha is the most commonly used solvent for this step, but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well. Remember when extracting, you want to swirl or gently mix the layers, not shake them. Nasty emulsions can form, which are to be avoided at all costs.
• Acid/Base Extractors – Now you need to deprotonate your DMT back to the freebase. This is done by adjusting your acidic extract to pH > ~9.5 . Typically this is done by adding sodium hydroxide depending on what pH you're aiming for. If necessary, the volume of the acidic solution may be reduced before basifying. The basic solution is then extracted with several volumes of nonpolar solvent. These extractions may be pooled unless you want to process them individually. The basic solution now theoretically been stripped of DMT, and can be discarded. There is some debate over the optimal pH for this step. It's known that with certain plants sources (like Chacruna), a pH of 9 is sufficient to achieve maximum yields. On the other hand, Mimosa extractors have found that a much higher pH is necessary; this is likely due to the effects of various phytochemical solutes on the polarity of the aqueous phase. In theory, the addition of excess salt to the aqueous phase of a Mimosa extract prior to defatting ought to accomplish the same thing as the tremendous excess of hydroxide, but I've not yet heard of this being successful.
• Straight to Base Extractors – Your solution is already basic, so you’re good to go on this step. Just extract your basic, bark-filled mixture with several volumes of nonpolar solvent. The volumes may be pooled or processed individually.
(Optional) Acid/Base Purification and Defatting
If you did an acid/base extraction, this step is probably unnecessary, especially if you defatted before recovering the freebase. It can be done if you’re really worried about impurities and aren’t partial to any of the subsequent purification methods. If you went straight to base, then this step could be worth your while, as it allows you to defat your extract. On the other hand, many people find that Mimosa has little enough fat content that defatting leads to an unnecessary loss of product.
Extract your nonpolar DMT freebase solution with several volumes of water acidified to pH 3-4 with your choice of acid (hydrochloric, acetic, tartaric, etc.) and pool the extracts. If desired, defat the acidic solution with a couple volumes of nonpolar solvent (naphtha, toluene, etc.). Basify the solution to regenerate DMT freebase and recover by extracting with several volumes of extracting solvent (naphtha, DCM, hexanes, etc.), pooling the extracts.
(Optional) Washing the Nonpolar Solution
Many teks don’t include this process, which comes from Vovin's Tek, but it seems to be the best option for those concerned about residual lye in the nonpolar phase. To neutralize any lye which still remains in your product, wash the nonpolar solution of freebase with a small volume of dilute sodium carbonate (washing soda), pH ~8.5 (this is not the same as baking soda, sodium bicarbonate). The layers separate easily without emulsion, so shake away, then drain the water from the bottom of your seperatory funnel (assuming you’re using naphtha so your organic layer is on top). Room temperature water should be used for the sodium carbonate solution to avoid cooling the naphtha and encouraging precipitation. If desired, you can perform a couple more quick washes with neutral (unbasified) water to remove any traces of the sodium carbonate which may have been left in the naphtha.
3. Recovering the DMT Freebase from Solvent
There are basically two schools of thought on this step: evaporate the solvent or precipitate DMT crystals by freezing. There’s nothing really wrong with simply evaporating if you’re going to be doing further purification on the material, but that being said, I still don’t really see any reason to do it until you’ve freeze-precipitated a majority of your product.
To freeze precipitate, separate the nonpolar solvent from the aqueous phase and place the nonpolar solvent in the freezer (with the temperature setting as cold as it will go), and allow it to sit overnight. Depending on how concentrated the solution is, a good portion of DMT ought to precipitate out as nice crystals. These crystals can be removed but must be dried quickly or in a cold environment, because they will redissolve as the solvent warms up. At this point your best bet is probably to reduce the nonpolar solution to something less than half its original volume, and freeze precipitate again. Repeat until no crystals result or the crystals have significant visible impurities, at which point you can either discard the remaining mess, or evaporate the nonpolar solvent and recover the last shreds of DMT by further purification. In a simple variation on freeze precipitation, some people report success in growing larger crystals by repeatedly transferring the recrystallizing solution back and forth between the freezer and fridge every few hours.
Now the only thing left to do is purify the loot.
(Optional) Wash Crystals with Cold Aqueous Ammonia (Not Recommended!!!)
This is a simple way to wash out some minor impurities and discoloration. Just set up a filtration apparatus, put the crude DMT on the filter, and rinse with a small volume of ice-cold aqueous ammonia (preferably 10% concentration). Many people have run into problem with this method, resulting in the ammonia dissolving away their product, making it difficult to recover.
(Optional) Recrystallize from Hot Solvent
This will help to reduce impurities and give the product a more sharply defined melting point, but it won’t do much to reduce discoloration unless combined with activated charcoal (see below). To recrystallize, dissolve your product in a minimal volume of hot solvent (e.g. roughly 20 mL naphtha per gram of DMT). This will probably leave an undissolved sludge at the bottom of the vessel; the DMT-laden solvent can generally be separated from the sludge by simple decanting. Allow the solution to cool slowly with minimal agitation. Once it has reached room temperature, transfer it to the fridge for a couple hours, then to the freezer. Though it’s not necessary, if you have a small DMT crystal on hand, you can add it to the solution to help seed the recrystallization. Regardless, a nice crop of crystals should precipitate out of solution, and can now be collected by filtration. If unsatisfied with the results of a recrystallization, you can always reheat the solvent to redissolve the DMT and reduce the solution volume, then repeat the cooling process. Naphtha is the most commonly used recrystallization solvent, but success has also been reported with hexane.
(Optional) Clean with Activated Charcoal
This seems to be the most effective and reliable method for removing discoloration. Proceed exactly as though you were recrystallizing, but after dissolving the DMT in hot solvent, add a small quantity of crushed activated charcoal and swirl occasionally, sustaining heat for about ten minutes. Decant the hot solvent from the charcoal and allow to crystallize as usual. This method generally removes only discoloration-related impurities and requires a fairly clean starting, which is why I don’t recommend doing it with the crude nonpolar freebase solution prior to the initial freeze-precipitation.
(Optional) Acid/Base Purification and Defatting
Unless your extraction was extremely messy and gave you a gunky mess instead of crystals, then this step is total overkill. If your product is a roughly crystalline solid, a wash with cold aqueous ammonia and recrystallization with activated charcoal treatment should clean it up just fine. But if you want to recover any DMT from the gunk you get evaporating your solvent after freeze-precipitating, this is the way to do it. Take up the crude material in water adjust to pH 3-4 with your choice of acid. Defat if desired, then basify, extract, and precipitate.
(Optional) Purify by Column Chromatography
Obviously this route is not for the average extractor, and assumes you have access to a chromatography column, or at least a buret which can function the same on a smaller scale. It is totally unnecessary unless you're aiming for analytic purity or you have a godawful extraction goo that calls for some heavy-duty purification. You may run a TLC first using the same solvent pair that you plan to run the column with to get an idea what you'll be up against, but this is probably not necessary. The DMT can be visiualized under UV light as a blue spot.
Plug the stopcock end of your buret or column with a glass wool (or less ideally, cotton) filter. Cover this with a small portion of sand and fill your column with silica slurry. Load your crude sample, and elute with your chosen solvent pair. Monitor the progress of the DMT with a UV light to capture the correct fraction. If you don't understand what any of this means, you probably shouldn't attempt it, but you can consult a lab manual to satisfy your curiosity.
Well, there you have it. If anyone knows of any other common or effective purification techniques, I'd be interested.
