User:Dmt brazil/manual
- https://wiki.dmt-nexus.me/The_DMT-Nexus_Extraction_Handbook
- https://wiki.dmt-nexus.me/DMT_Extraction_Overview
- https://wiki.dmt-nexus.me/FAQ#Where_to_start.3F
- https://wiki.dmt-nexus.me/w/images/0/09/The_DMT_Handbook_201208.pdf
- https://wiki.dmt-nexus.me/Straight-To-Base_Extraction
- https://wiki.dmt-nexus.me/Acid/Base_Extraction
- https://wiki.dmt-nexus.me/Dry_Technique_Extraction
- https://wiki.dmt-nexus.me/Limtek_Extraction
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?
Acids and Bases
A proton is a positively hydrogen ion, H[sup]+[/sup]. 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 (CH[sub]3[/sub]COOH) gives up the proton on its -COOH group (incidentally, this is called a "carboxylic acid"Pleased, its conjugate base is the acetate anion (CH[sub]3[/sub]COO[sup]-[/sup]). Thus acetic acid and acetate are called a "conjugate pair". Likewise, every base has a conjugate acid; for example, when ammonia (NH[sub]3[/sub]) aquires a proton, its conjugate acid is an ammonium cation (NH[sub]4[/sub][sup]+[/sup]). (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 (CH[sub]3[/sub]COO[sup]-[/sup]), 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.
Universal of extraction 2
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, but calcium carbonate or calcium hydroxide can also be used, 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 and the extractions pooled. 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 and pool the extracts.
(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, put your 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) and 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.
Extraction
Extraction generally refers to the process of isolating a product from a source. The basic idea is to utilize the unique properties of the product—whether reactive, electromagnetic, or otherwise structural—to draw it out of the source and into a target solvent. To accomplish this the product must either be naturally soluble in the solvent or must undergo reaction to increase its solubility. The difference between a high and low yield is firstly determined by how much more soluble the product is in the target solvent, than in its source material or solution, and secondly by how thoroughly the target solvent is mechanically brought into contact with the target solvent; this is generally determined by a combination of the droplet size and dispersion of a solvent and/or the surface area exposure and structural consistency of the source material.
See also:
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Straight-To-Base Extraction
Straight-To-Base or STB techniques are generally considered the simplest of extraction techniques and, as such, are the most commonly used. The process involves the use of a strong base reagent in solution to break down source material and convert the contained product from its natural salt form to freebase, which will in turn be more soluble in an NPS than in the basic aqueous solution.
Considerations:
- The use of "Straight To Base" techniques requires little experience or technical know-how for beginners to approach extraction techniques. STB is best-suited for quick, non-labor-intensive, crude bulk extractions. It requires no straining or cooking but requires time for soaking and separation. STB tends to yield a greater array of botanical impurities due to its lack of straining and defatting. These techniques do however enable a more thorough exhaustion of product from the material. This technique is ideal for shredded material that requires little or no defatting.
Overview of Materials and Methods
materials_list
- DMT-Containing Material Requiring no Defatting
- NPS
- Water
- Strong Base
- Typically Lye
- Chemically Resistant Vessel to Facilitate Reaction and Agitation or Stirring
- Separatory Device
Material Considerations
- Lye is extremely toxic and hazardous, though most find it easy to handle safely.
- STB methods generally demand a hefty volume of solvents for sufficient performance.
- Naphtha and heptane are generally found to pull a more pure product, and though their poor ability to dissolve DMT demands some amount of heating to pull a considerable amount, it also allows for product to be isolated by freeze-precipitation.
- Toluene and Xylene are generally found to dissolve DMT more easily but also dissolve a wider range of alkaloids and other substances from the source material, and though they do not facilitate freeze-precipitation, they do facilitate the use of FASA.
- DCM is capable of pulling an even fuller range of alkaloids from the source material, as unlike other NPS's, it sinks in water.
- Diethyl ether as a binary solvent in combination with heptane also pulls full-range alkaloids. Using this combination the ether can be distilled off rather rapidly, leaving behind an alkaloid-saturated solution of heptane ready for immediate freeze precipitation. Note! Diethyl ether is extremely flammable. Exercise extreme caution!
- Limonene has become the solvent of choice among many--largely due to being nontoxic--but is considerably more expensive and harder to find than other less savory NPS's, and though it does not facilitate the use of FASA or freeze-precipitation, it can facilitate salting methods like FASW and FASIPA.
- Most commonly used solvents do not facilitate expedient or clean evaporation, due to either impurities from the solvent itself or pulled from the source material, though heptane and naphtha tend to be most effectively used in this way.
Methods:
- STB extraction involves a soak of pulverized source material in a basic solution, followed by the stirring in of an NPS. The NPS is separated from the aqueous solution by siphoning, pipetting, or use of a separatory device.
Material Preparation
For standard STB, the source material must generally be at least shredded, though preferably powdered. It has been found beneficial to pre-treat the pulverized material with an acid soak, with or without heat, prior to immersing in a basic solution.
Extraction Procedure
- Prepare a basic solution between pH 12-14 by adding base to the appropriate amount of water for the amount of source material to be used.
- Immerse the pulverized source material in the basic solution and allot time for material breakdown and freebase conversion.
- Stir or shake in the target solvent enough to ensure adequate dissolution of product.
- Allow the solvent to separate from the aqueous solution in two distinct layers and separate using appropriate separatory methods.
- Collect solvent and proceed with appropriate desired crystallization methods.
Further Elaboration and Technical Support
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Acid/Base Extraction
Acid/Base or AB extractions use a weak acid(citric, acetic, and OTHERS have been used with success) to extract the DMT from the plant material into DMT freebase.
Considerations:
- The use of Acid/Base techniques implies the use of "acid-cooking" the source material, straining it, and basifying the resulting strained solution. The use of an initial acid extraction facilitates the implementation of a defatting phase and generally yields a product more devoid of botanical impurities. This technique is ideal for any material that requires defatting, though defatting may not be necessary, depending on the intended method of crystallization.
Overview of Materials and Methods
Material Preparation
Either purchase shredded bark or Break 1-Pound of Mimosa Hostilis rootbark into 2" pieces and grind it all up in a glass-topped blender, a little at a time.
Extraction Procedure
(taken from tek) Premix in an empty 1-Gallon plastic jug: 1-Pint White Vinegar & 3-1/2 Quarts Water. Put the ground up Mimosa in a 3-Liter crockpot, then fill it with the water-vinegar solution.
Stir well and turn it on "high". After 2 hours, remove the crockpot ceramic liner, hold the lid on slightly offset, and pour off most of the liquid into a 1-gallon wide-mouthed glass or stainless container.
Add the remaining water-vinegar solution to the crockpot again. Stir well and turn it on "high". After 2 hours, remove the crockpot ceramic liner, hold the lid on slightly offset, and pour off all of the liquid into the same container again. Discard the rootbark fiber and save the two combined extractions in the 1-gallon container.
Allow the vegetable particles in the extraction in the 1-gallon container to settle to the bottom overnight. Then pour off the liquid into an empty 1-Gallon GLASS wine jug, being careful not to pour off any of the vegetable sludge at the bottom. Discard the sludge and keep the contents of the wine jug.
Premix in advance a solution of: 4 Tablespoons (50grams) of Sodium Hydroxide ("Red Devil" lye) with 1-Pint of HOT Water. Stir well. Slowly add this solution to the wine jug, then cap the jug. Gently tilt the wine jug back and forth for 1 full minute to mix the contents.
from here use your solvent of choice
Further Elaboration and Technical Support
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Dry Technique Extraction
Dry techniques (drytek) evolved from and are ideally intended for the implementation of the FASA method of crystallization and serve as the only techniques able to implement acetone as an extraction solvent. Acetone is generally favored for its ability to extract a notably broad range of active products.
Considerations:
- The use of dry techniques requires fewer and less toxic materials than the techniques that employ aqueous phases and separatory methods. The materials required are generally of a more household nature. They are most effectively applied to powdered botanical material. Acetone is, however, completely water miscible, so proper drying procedures are of the utmost importance. This technique may or may not require the defatting of botanical materials, depending on the intended method of crystallization. Dry techniques are the youngest of the current extraction techniques though apparently sound in theory and in practice.
Overview of Materials and Methods
materials_list
- Powdered DMT-Containing Botanical Material
- Water
- Acetone
- Magnesium Sulfate (Epsom Salt)
- Household Base:
- Either Sodium Carbonate (Washing Soda)
- or Calcium Hydroxide (Pickling Lime)
- or Sodium Bicarbonate (Baking Soda)
- Only after Conversion to Sodium Carbonate
Material Considerations
- Acetone can be purchased at hardware stores but should be confirmed as pure acetone prior to purchase. Note that almost all acetone can contain up to 5% water contamination, depending on time and shelving conditions.
- In order to be utilized for extraction, sodium bicarbonate must undergo conversion to sodium carbonate.
- Lime is often found difficult to decant acetone off of and also difficult to filter out of acetone, whereas sodium carbonate is generally found more agreeable for both.
- Distilled water is preferable, as tap water almost always contains impurities that can potentially tamper with resulting yields.
- With few exceptions, the source material should be completely pulverized to a powder consistency before use, as this technique's choice of reagents are not quite capable of penetrating cell structure.
Methods:
- Extractions by dry techniques are characterized by the lack of a traditional aqueous phase in the extraction process, and instead, opting for basification within a paste which is followed by chemically drying the paste with desiccant. The process does not make use of separatory methods, and instead is characterized by it's use of dry-washing, decanting and non-intensive filtering methods. Certain materials must be rendered anhydrous prior to use.
Material Preparation
Rendering Anhydrous Magnesium Sulfate Rendering Anhydrous Acetone Conversion of Sodium Bicarbonate into Sodium Carbonate
Extraction Procedure
- Mix the intended base with the powdered source material at a ratio between 1:2 and 1:1.
- The product remains in its natural salt form which is generally considered to be quite free from the botanical cell structure in powdered material.
- Add only enough water to thoroughly moisten the mixture to the consistency of a paste while stirring to ensure the consistency of the mixture.
- Although this is not generally considered a traditional aqueous phase in that it is not a solution, it is an aqueous phase in that it is excessively hydrated and sufficiently aqueous to facilitate reaction.
- Allow adequate time to soak in order for reaction to occur.
- The acid component of salt-form product undergoes reaction with the base, effectively neutralizing the acid and freeing the product in its pure alkaloid form, or freebase.
- Stir in anhydrous magnesium sulfate until thoroughly dry.
- The magnesium sulfate acts as a desiccant, and that this is performed in order to prevent water contamination of the acetone.
- Add an excess of anhydrous acetone and stir thoroughly, allotting adequate time and stirring for thorough dissolution of the product into the acetone.
- The more contact allotted between the product and the acetone, the greater the saturation.
- Decant and/or filter acetone and collect, being careful not to allow any particulates into the collection vessel.
- The bases used should not harm the quality of the product, but may interfere with the accuracy of weight.
- Repeat steps 5-6 with fresh acetone until material is exhausted to satisfaction, and proceed to the appropriate desired crystallization method.
- Three washes is generally considered sufficient.
Further Elaboration and Technical Support
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Limtek Extraction
Though all of the other extraction techniques may be employed in nontoxic or at least less toxic manners, few are perfectly suited for completely nontoxic implementation with food-grade household chemicals. Limtek extraction is named as such because it employs the use of d-Limonene and pickling lime, and is distinguished by the unique way in which lime must be used for effective results--similarly to drytek--as well as the hygrophobic properties of limonene. Unlike most bases used in extraction, lime has very low solubility in water, and so even though it does qualify as a strong base, it does not behave as such in solution; it must be mixed into a paste with the source material and a minimal amount of water in order to behave as a strong base. One of the drawbacks of drytek extraction is that upon removal of moisture from the mixture of material and reagent, the reaction will essentially terminate, greatly limiting the effectiveness of the extraction. Limonene, however, is an NPS and so is hygrophobic, meaning that the source material can remain moist.
Considerations:
- Limtek extraction is nontoxic and food-grade throughout, using no toxic or otherwise hazardous materials in the process. This technique uses the absolute minimum of material and volume possible for extraction, and due to it's lack of a proper aqueous phase in the extraction process, requires no separatory methods prior to salting and facilitates solid disposal in lieu of dumping large volumes of potentially toxic solution. This process bears the least resemblance to the production of other less savory substances, reducing legal risks to the operator, to include chemical odors.
Overview of Materials and Methods
materials_list
- DMT-Containing Botanical Material
- Water
- NPS
- Typically d-Limonene
- Calcium Hydroxide (Pickling Lime)
Material Considerations
- In order for the process to remain nontoxic, an aqueous food-grade acid should be used to salt out of the product.
- FASW (Fumaric Acid Saturated Water) can be evaporated to achieve a crystalline DMT fumarate.
- vinegar can be used to achieve DMT acetate but will not crystallize.
- Limonene can be replaced with other NPS's, but the process will cease to be nontoxic.
Methods:
- Extraction by limtek is characterized by the lack of a proper aqueous phase but also the lack of necessity for drying procedures, and essentially involves a pasty or doughy material being washed in the target solvent to retrieve product.
Extraction Procedure
- Mix the powdered material with lime between 1:2 and 1:1 and mix thoroughly.
- no reaction occurs at this point but thorough mixing will help to ensure an even reaction for the following steps.
- Thoroughly moisten the mixture while stirring, ensuring that no dry spots remain and the mixture exhibits a doughy or pasty consistency.
- the added water facilitates reaction and a basic environment which may aid in breaking down the plant material.
- the acid component of the natural salt-form of the product within the plant material will be neutralized, yielding a freebase product.
- Ensure a thoroughly homogeneous mixture and allot enough time and stirring for a complete reaction.
- this is the most important part for a successful yield, and due to the lack of a proper aqueous phase, the reaction requires a stronger degree of manual facilitation.
- Wash the mixture with NPS by stirring and decanting to collect the NPS, and proceed to the appropriate desired crystallization method.
- the more contact brought between the material and the target solvent, the more successful the extraction will be.
Further Elaboration and Technical Support
- Directory of Current Limteks
- A Poll to Gauge Members' Success w/ Lime
- Pickling lime instead of lye?
- Calcium Hydroxide instead of lye?
Crystallization
Crystallization is the process by which a product is isolated from a solvent. This is accomplished by either allowing the solvent to completely evaporate or by causing a precipitation to occur within the solvent, which can then be isolated from the solvent by several methods and then dried of any residual solvent.
Evaporation and Slow Precipitation
In extraction, evaporation is the process by which a solvent disperses from its liquid form into the air as a vapor and a gas. When this occurs, the less volatile constituents of the solvent solution are left behind, and as such, it is a common method of isolating solutes from solvent. Typically, a solvent is evaporated in a shallow dish in order to maximize surface area exposure, often with mild heat and airflow applied to hasten the process; however, minimizing surface area and airflow and eliminating heat are often found to improve the quality of precipitate yielded by process of slow precipitation. Many solvents are found to be limited in their ability to crystallize a product by evaporation, yielding a product ranging from oils and "goo," to waxy crystals, to fluffy crystalline powder, to hard crystal shards. These discrepancies in quality of yield are determined by the solvents speed of evaporation, solubility of product in the solvent, or impurities present in the solvent.
Considerations:
- Many common solvents contain impurities which may not be quite as volatile as the pure solvent and may leave these impurities behind as a residue.
- Solvents often emit fumes and odors which may be hazardous to health, flammable, or may alarm those within proximity of the odor.
- Some solvents may require an excessive length of time to evaporate.
- Some solvents may absorb ambient moisture, resulting in a less expedient evaporation.
- Excessive air flow may cause the oxidization of the product.
- Solvent may become Trapped within the crystal structure of the product, resulting in a less solid and less pure product.
Full-Range Extracting Solvents
Low-Solubility Solvents
Theses solvents dissolve a much more narrow range of product and are used to isolate DMT from active and inactive impurities, alike. However, when used for extraction, they are often heated and dissolve a bit more variance in alkaloids, and they may require further purification.
- Heptane requires much heating to dissolve any significant concentration of product but precipitates product very easily at room temperature or cooler. It is often found in quite pure form, reliably free of additives, and is a choice solvent for recrystallization and slow evaporation and precipitation.
- Naphtha can require a bit of heating to dissolve a significant concentration of product but precipitates product relatively easily at room temperature or cooler. While never without a wide variety of additives, some brands will evaporate cleanly without leaving a residue. This is a common solvent used for both extraction and evaporation but is often considered most preferable for freeze precipitation.
Polar Solvents
Salting
Salting is the process by which freebase DMT is reacted with an acid to create a salt form which is generally water-soluble. The natural form of DMT in botanical sources tends to be a salt-form, thus facilitating the simple aqueous extraction used to prepare DMT-containing brews. It is quite common to perform aqueous acid extractions from the material, however—whether for the purposes of a brew or for A/B extraction. The salt-form itself rarely lends itself to proper crystallization and usually can only be isolated as an oil unless very specific methods and materials are employed.
The Use of Fumaric Acid
Few salt-forms of DMT facilitate crystallization, but DMT fumarate currently stands alone as a solid crystalline salt-form of DMT.
The FASA Method The FASW Method The FASIPA Method
Discussion of Other Salt-Forms
Further Elaboration and Technical Support
Purification
The purification of DMT product has several purposes and is accomplished by several different methods, but all of them essentially involve the washing of product in some way or another. Purification either involves the isolation of product from unwanted impurities from the plant source or from the process of extraction, or it involves the isolation of product from active impurities which may or may not be collected after isolation.
Recrystallization
The general purpose of recrystallization is to crystallize the product in a fresh solvent after it has already been isolated from the extraction solvent, likely containing a considerable amount of impurities. In this technique, an impure solid compound is dissolved in a solvent and then allowed to slowly crystallize out as the solution cools. Often this process results in more well-formed crystals with less discoloration. The advantage of this method of purification is that the solvent choice for recrystallization may be different and more suitable than that chosen for extraction. Crystallization of a solid relies on slow, selective formation of the crystal lattice and is quite different from precipitation. In freeze precipitation, there is a rapid formation of a solid from a solution that causes impurities to be trapped within the solid's crystal framework. For this reason, extractions that rely on precipitation or evaporation to produce a solid product always include a final recrystallization step to give the pure compound.
The process of recrystallization relies on the property that for most compounds, as the temperature of a solvent increases, the solubility of the compound in that solvent also increases. For example, much more sugar can be dissolved in very hot water (just below boiling) than in water at room temperature. Inversely, if a hot saturated solution of sugar and water is allowed to cool, sugar will begin to crystallize out of solution as solubility decreases. Recrystallization will give your product a more sharply defined, uniform melting point and in the case of DMT allow for hard non-waxy crystals.
Finding a suitable solvent
The first consideration in purifying a solid by recrystallization is to find a suitable solvent. A good recrystallization solvent should fit the following criteria:
1. The compound should be very soluble at the boiling point of the solvent and only sparingly soluble in the solvent at room temperature.
2. The unwanted impurities should be insoluble in the hot solvent.
A good recrystallization solvent for DMT is heptane. DMT is not very soluble in it at room temperature but quite soluble as we add heat. Most common spice impurities, however, are not very soluble in it at all and can thus be separated via simple decanting.
Dissolve solid into hot solvent
Prepare a waterbath and heat the DMT and the heptane in their own beakers until the DMT begins to melt. Add heated solvent dropwise into the beaker containing the extract. The heptane will go cloudy almost immediately and take on a yellow color as the DMT goes into solution. Keep adding heated solvent until further addition or agitation causes no more DMT to dissolve.
Your beaker should now contain yellowish-tinged heptane with an orange-brown blob of oil and undissolved solids at the bottom of the vessel. Carefully decant the solution into another beaker, careful to leave the impurities behind. Repeat dropwise addition of heated solvent and decantation to ensure no DMT is left behind.
Decolorize with carbon
Now that we have dealt with insoluble impurities, our solution is see-through but tinged yellow. This discoloration is due to the presence of high-molecular-weight reaction by-products which may have been formed during the extraction process. A simple wash with activated carbon will get rid of decolorizing compounds. (Activated carbon is extremely efficient at absorbing impurities due to its large surface area.)
1. Add excess solvent and activated carbon, and boil the solution for a few minutes. The colored impurities will adsorb onto the surface of activated charcoal.
2. Remove the charcoal with absorbed impurities by filtration. Your solvent should now be almost clear. If the yellow color persists, repeat the charcoal wash carefully.
Note: Very little activated carbon is needed to remove the colored impurities from a solution. You must be careful in your use of decolorizing carbon: if too much is used, it can adsorb the desired compound from the solution as well as the colored impurities.
Crystallization
After the solution has been filtered cover the flask containing the hot filtrate and set it aside undisturbed to cool slowly to room temperature. As the solution cools, the solubility of the dissolved compound will decrease and the solid will begin to crystallize from the solution. Once the solution reaches room temperature, move it into the refridgerator, and finally into the freezer to freeze precipitate most of the DMT.
The slower your solution cools, the cleaner and larger your crystals will be.
Further Reading
How to Crystallize Organic Compounds - WikiHow
Recrystallization Technique - Rhodium
Freebase Conversion from Salt
The methods used for converting crystalline salt-form DMT into freebase are not dissimilar from those used in extraction. The only significant difference between the processes is that the conversion involves far fewer impurities and less material than the extraction. Because of of this and the fact that it involves the isolation of the product from an acid, the conversion acts as a sort of purification method.
Drytek Freebase Conversion of DMT
Crystalline Freebase Conversion of DMT
Nontoxic Freebase Spice Conversion
STB Freebase Conversion of DMT