Version 0.5
Last modified: 1 August 2003
Copyright © 2003 Elfspice
This document is licensed for redistribution under the GNU Free Documentation Licence
When modifications are made, put credits below this line.
Revised in March 2005 by Loki Contents
WARNING (READ THIS FIRST)
Acknowledgements
Introduction
The Plant
Equipment and Chemicals
Step 1 - Prepare the Bark
Step 2 - Acidification and Aqueous Extraction
Step 3 - Non polarwash (Defatting)
Step 4 - Basify to pH 13
Step 5 - Non polar Extraction
Step 6 - Polar Wash
Step 7 - Evaporate Non polar Extraction
Step 8 - Recrystallisation Purification
Conclusion
Appendix
Extraction Reports
Changelog
WARNING
Something that was drawn to my attention regarding the content of this document was that there is no warnings about the materials discussed with regards to the dangers and effects of the materials produced, and not enough about the warnings about some of the chemicals used (in particular, shellite/naptha and sodium hydroxide).
ABOUT DMT
DMT is widely regarded as the most potent psychedelic drug known. As has been said by someone else, the term 'mind blowing' could have easily been invented to describe this drug. It is not a 'high', or a party drug or any such thing.
To briefly sum up some of the sorts of nasty experiences that a person can have under the influence, it ranges from an experience of dying, being torn apart by vicious animals, being probed and having strange implants installed by cold uncaring aliens, extreme experiences of humiliation...
Now, after reading that list, one might wonder why a person would be interested in using this drug at all... Well, basically, because things completely off the other end of the scale can also happen during the experience. Contact with happy elves or clown-like entities, exchanges with entities who wish to teach you something, healing experiences, positive contacts with aliens.
The way it affects people is extremely idiosyncratic, but I can say one thing that is common to all experiences - it is always humbling, the awesome potency of this drug should not be underestimated.
MONOAMINEOXIDASE INHIBITORS (MAOI's)
The use of monoamineoxidase inhibitors, such as syrian rue, banisteriopsis caapi or synthetics such as moclobemide, which is a common way to activate oral doses of DMT, should be done with great caution. There are elements in most people's diets and drug intakes which, when combined with the use of MAOIs can lead to a serious medical emergency if proper precautions are not taken prior to ingesting MAOIs.
Monoamineoxidase inhibitors (MAOIs) should not be taken in if any stimulants (caffeine, amphetamines, cathinone, methcathinone), or SSRI antidepressants (prozac, citalopram, zoloft etc) have been taken less than 48 hours beforehand, the same goes for beer and wines, and there are foods which contain proteins which are dangerous if consumed within the same period of time, these are generally aged protein products (wurst, jerky, salami) and yeast-based products, such as yeast extracts, wines, beers and other brewed or fermented materials.
Bread is not so bad, since the yeast is still fairly fresh when it is eaten, but at least 12 hours should be witheld to avoid problems. The main issues are aged proteins, which covers brewed alcohols, aged protein foods, and SSRI's and amphetamines are contraindicated, though the info on the dangers regarding MAOIs mainly applies to synthetic MAOIs (eg moclobemide).
I have been told that syrian rue and harmala do not cause significant risk with amphetamines and fresh yeast products, however they do potentiate amphetamines. It is best to avoid them if you are unsure or have not done small scale tests to ensure it is safe...
In most cases, one will only get a nasty headache, but it is best to avoid any of these things with MAOIs, recently a teenager made CBS news from mixing a MAOI with something of this nature (and of course the news people, not really interested in the propagation of safety information, didn't say what it was that caused the problem, however it would have been one of the above, as you can see it covers a lot of common foods and drugs).
What happens is the MAOIs prevent the action of the monoamineoxidase by preventing it from being synthesised, which stops these enzymes from breaking down chemicals in the brain and blood to prevent their levels building up too high.
The natural cycle in plasma is of precursors, such as amino acids, being synthesised into neurotransmitters by enzymes, and these neurotransmitters only have a limited useful life in the blood as free radicals and other agents can break them and cause toxicity problems (which is the suspected but not officially recognised cause of people going bezerk on prozac), and so they must be removed after a certain amount of time.
Also a number of chemicals cause dramatic changes in physiology, such as stimulants, and the amine tyramine, found in aged proteins, which is a product of yeast I believe, and the monoamineoxidase enzyme is responsible for protecting us from this toxicity.
When an incident occurs with MAOIs, a mild incident will involve a headache, but if too much poisons are in the blood when the MAOI is ingested, they remain active, and what is called a 'hypertensive crisis' occurs. This means severe headache, high blood pressure and heart rate. If the blood pressure gets too high, a stroke can occur, and beyond that, death from major brain haemorrhage.
SAFETY WITH CHEMICALS
In this document are described the use of numerous chemicals, the ones of most concern are the Non polar solvents (naptha/shellite, toluene, xylene) and sodium hydroxide.
I recommend the use of solvent resistant gloves whenever contact may be had with the solvents. One should be able to find nitrile gloves in the supermarket, they are marketed as 'non allergy', some people are allergic to latex apparently (personally I hate latex anyway, it makes my eyes red). Nitrile is functionally equivalent for this process as neoprene, however neoprene is much more durable and as I discovered a little while ago, nitrile decomposes when in contact with acetone for an extended period of time.
No sources of flame or sparks should be present when working with all nonpolar solvents, and one should take care to avoid inhaling the vapours as much as possible. Always work in an area with good ventilation when working with shellite/naptha, hexane, toluene or ether.
I have personally been burned by an explosion with shellite, it was only second-degree (the skin was fully damaged, but it hadn't gotten down to the flesh). I was in pain for three days, constantly spraying it with xylocaine spray to stop it from being so painful I was unable to fall asleep. It also put carbon all over the space that it exploded in.
This was from inadequate ventilation and a spark from moving a pot around on an electric hotplate while blowing the vapours out of the pot. The vapours of shellite/naptha are heavier than air, so they will fall downwards, so it is particularly crucial that there is nothing incendiary below any amount of such materials at close to it's boiling point.
The vapours will also flash back to the source of vapour for quite a distance, at least two metres clearance should be given before anything with a slight risk (including a mobile phone) of causing a spark should be permitted nearby. It is also for this reason that, unlike numerous other guides, I don't recommend heating the solvent when extracting. Besides everything else, experience tells me that one does not need to increase the solvation power of 300ml of naptha to get everything desirable out of an expected 1-3g yield. The only time when it is sensible to heat naptha is when recrystallising, and this can be done in open space using boiling water from a jug.
Sodium hydroxide (NaOH) is also very dangerous, anyone who has seen the movie 'Fight Club' would recall the scene where Tyler Durden puts a pile of this material onto the protagonist's hands. When it comes into contact with water it reacts with a very strong exothermic reaction (it generates heat), and for this reason the NaOH should always be added to water and not the other way around as this ensures that the heat is absorbed by the water, rather than the heat inducing the hydroxide to react violently with the humidity in the air, and it can in fact explode, spraying highly reactive material everywhere, and when this gets on the skin or in the eyes, it burns severely.
It is recommended when working with sodium hydroxide to wear protective goggles in case it splashes in the face, it can destroy your vision .
Acknowledgements
I would like to acknowledge the contributions of various people who have helped me gather the information I have assembled in this document. Thankyou to Yjanni, Mescalito Ted, Yoda, Quantum Tantra (for her wonderful guide), Meme (for the recrystallisation information and for sharing my passion for improving techniques and administration), Carpedmt (for highlighting the fact that extractions do not need take a long time, and for introducing me to acacia obtusifolia), Silicon7 (for his knowledge of proper chemistry procedure and help with materials), and his cat Moofie who's presence in the lab greatly amused me.
Rhodium (who's excellent chemistry knowledge and great information resource http://www.rhodium.ws and the hive http://www.the-hive.ws) (R.I.P. rhodium and the hive), Gastro (who provided my first few quantities of acacia extract many years ago), Mulga (for his very informative and useful site), Mesqualero (for moral support and for inspiring me to create a more clear format for the instructions and notes), Andrew (for his report), Eccles for his excellent pKa info on DMT, Glorfindel (for pointing out the need for pH 12.5 or higher for polar washing which, sadly are a bad idea as it turns out), Gumby, for emphasising the safety factors.
Bluetonguedragon for his encouragement, Ion for his excellent explanation of eliminating tannins and dry extraction techniques (which I don't explain here), all the people who have emailed, pm'ed and instant messaged me with praise for this, and anyone else who I have gathered information regarding this process who I might have forgotten.
Introduction
I have written this guide to specifically cover the process of extracting alkaloids from the Acacia Obtusifolia tree's bark, which is the most consistently yielding of the acacia species with regards to it's yield of psychedelic tryptamines, primarily N, N Dimethyltryptamine .
It is equally applicable to mimosa hostilis, and is likely to be useful for any other DMT source contained in the bark of a plant (eg, desmanthus illinoensis, mimosa hostilis). Chlorophyll laden sources, such as phalaris and psychotria viridis et al have not been studied by the author, however at some point in the future the special considerations for these leaf materials will be added. These other materials very likely will need other measures or perhaps more focus on washes.
One thing that I have learned in recent months about the process of extracting alkaloids is that the long periods of time suggested in older guides are unnecessary, this suspicion started to come to me when I witnessed the acid/base extraction of alkaloids from an alkaloid synthesis and saw that the alkaloids can in fact cross phases in a matter of minutes, not hours or days.
Taking care to ensure certain pH levels are used also eases and improves the process, specifically in the acid phase the pH is better if it is about 4, and in the extraction less emulsion problems occur when working with a pH above 12.5 (sodium hydroxide does not raise the pH above 13.5 when diluted 5g/100ml, so the concern about 'pH spikes' is unnecessary so long as the base is diluted).
When washing and extracting, use gentle agitation rather than violent, swirl, stir or turn it end over end gentlyrather than shaking it. Water washing is less of a problem in this respect, usually by that stage the majority of emulsion causing chemicals have been removed. Excess sodium hydroxide can cause problems however - the best policy is to only add it as much as is required to achieve around 12.5-13 and stop there.
Something else which I have heard from others, which I have now verified, is the value of doing washes. Previously washing was little mentioned, and only the wash of the acidic extract was suggested (and again, a much longer than necessary time stated), when in fact the best results seem to be from doing a non polar wash of the acidic extract, and using a fairly low pH (like 8-9) and no salt, for washing the non polar extract (the best proceedure seems to be using sodium bicarbonate as it reacts with sodium hydroxide to produce sodium carbonate, which more readly comes free of the nonpolar fraction).
Washes ensure the resulting product is as free from contaminants of a non-alkaloidal nature as possible, in particular residuals of the base being used. Again, gentle agitation is completely sufficient for extractions and washes, and in the case of water washes, violent agitation will not allieviate suspended droplets of the base, the bubbles of the wash water, being alkaline, will wash some out, but will also leave the suspended bubbles of base in the nonpolar solvent, though by this stage in the process it doesn't matter as much as it should be quite clean already.
Finally, the best methods for recrystallising the product seem to be coalescing for me as well, I will talk about this at the end, the purpose is not, properly speaking to make pretty rocks, though if large crystals are produced they have a longer shelf life due to lesser surface area per volume, but instead, the purpose of recrystallising is to eliminate the contaminants in the solvent commonly used (naptha), as well as reducing other contaminants. This requires slow cooling or progressive cool/warm steps.
Getting a better degree of purification from recrystallising can be achieved by following the initial naptha recrystallisation with a recrystallisation in isopropyl alcohol or ethanol. The method required to do this has been added to the recrystallisation section.
This guide will not attempt to cover the extraction processes for other plant materials, however it is intended to be comprehensive and to the point, and should apply more or less to other materials, assuming one aims to result in a freebase, and the alkaloid in question is fairly similar in chemical characteristics.
I will also focus on the equipment which will ensure the best results with the least outlay without any compromise of efficacy of the process.
The Plant
This guide is specifically targeted at the acacia obtusifolia, I cannot really enlarge upon other information already available through libraries and on the internet, but I intend to replace this section with a comprehensive guide to finding them based on a series of expeditions to likely locations and lots of photographs, and, of utmost importance, in plain english.
One of the problems with the botanical information regarding these plants is that they never go into much detail about the bark structures. When walking through a well developed forest, quite often the tree is so far above you that you can't see a thing of what they describe in the botanical description.
As soon as possible, a photographic expedition will be made to bring back good photographs of the plant in it's mature natural state. The full extent of the obtusifolia's habitat is not fully known, it may well be more common than is currently thought.
The guide should be applicable to other sources of DMT, as the method described is very thorough.
Equipment and Chemicals
Other, more advanced chemistry equipment can be used for this process, however my aim is to only talk about what I believe to be the minimum standard to ensure the best possible results.
1.
Large Cooking Pot - for beginners it is wise to start small, 2-4L soup pots are good for this. Do NOT use aluminium pots for this stage, even organic acids will take up some of the aluminium oxide on the coating and the aluminium will react with strong acids to produce aluminium salts (eg aluminium chloride) and this is not something that one wants to need to get rid of, let alone ingest. (Mind you, it has little chance of getting into the product unless one does not do the aqueous wash).
2.
Glass Baster - this is a large pipette used to suck up oils from fowl being roasted in the oven and coating them so they get nice and golden crispy on top. A baster has a long glass tube and a rubber squishy thing at the end and it works like a dropper. Generally they can hold about 30-40ml. Glass is essential because these devices can be used to separate immiscible phases. These devices are available at most kitchen shops.
I just want to emphasise again - make sure it is glass - some of the solvents used will attack plastics (especially nylon, which is the common plastic baster material because of it's high melting point) and metal is completely useless for this purpose.
Also it is good if the device has a tip on it which is very narrow for half a centimetre or so, this improves this device's ability to precisely separate fractions and how well it holds the fluid when removed when held mid-air.
If you are willing to ask around and look around on the internet, you can find polypropylene separatory funnels, for around US$20 which are at no risk of breaking and allow one to separate phases much more rapidly.
3.
pH Measurement - In my opinion it is worth the money to get a good pH meter. These can be purchased from hydroponics shops and aquarium shops, they are commonly called 'pH Pens' or something similar. When getting a pH meter be sure to get an ample container of pH 7 'buffer' solution for calibrating it, and do this at least once a month.
pH papers can be used, however the extract has a very dark reddish colour and stains the papers. The only type of paper test which is suitable is the type with four different tests on each strip, and the reason why I suggest using an electronic tester is that dollar for dollar, it is hard to see what the effective advantage is, for the cost of 400 strips one can have an electronic one, and the electronic testers are accurate (if calibrated correctly) to about ±0.05 pH units.
Though this is not critical, using precisely measured pH levels every time is helpful in generating consistent results as the exact pH levels influence solubilities of various constituents of the plant material, and the best policy is to try and pick a pH which dissolves what you want and as little of what you don't want.
Bear in mind that every extraction requires about 10 individual pH tests, thus for the same money as you can do 400 extractions with paper tests, you can do well over 1000 with a pen. *** The pens usually do not stand up very well to nonpolar solvents, they don't really damage the sensor but they damage the case. This can be avoided by taking care to ensure as much of the nonpolar is removed as possible.
Note that one can get by in this process without a pH meter, but it helps ensure results are more consistent. Overbasifying and underacidifying both can cause problems.
4.
Large Jar - a jar like the ones that cranberry juice is sold in is perfectly suitable for the task, though a 2L canning jar can serve quite well also. If a canning jar is used, it should be tested with turpentine to ensure that the rubber used on the seal does not get damaged by it.
The juice bottles also have the advantage of being able to rapidly vent, the clips on canning jars require much more time to open when venting. Shellite is safe to use with most common HDPE plastic bottles, and is suitable for xylene and toluene as well (but plastic bottles are not suitable to work with hot liquids).
An empty shellite bottle is suitable also. This is the container that the extractions and washes will be done in, so it needs to be as large as the quantities of material you work with, and the opening big enough to permit the use of the baster.
5.
Colander - to catch bulky fibrous material from the acidic extract .
6.
Strainer - This will catch the larger particles.
7.
Fine Strainer/Tea Strainer - this will catch medium sized particles, which will block the coffee filters.
8.
Cotton, Acrylic or Polyester felt - common pillow stuffing can be used here, so long as this is done before doing the Non polar washes.
This material catches a lot of fine particles, it functions as a 'depth filter', which is a thick filter which is used to remove the majority of large and medium sized gunk before using filter papers. This kind of filter will also be helpful with the gunky gooey materials that are sometimes present.
9.
Coffee Filters - to filter finer particles out of the solution. Particles of bark will make seeing the line between phases in the Non polar wash difficult to see. The coffee filters can be good for removing hairs and other junk when recrystallising as well.
If one really wants to take ultimate measures to ensure the elimination of particles, scrolling up unscented toilet paper or kitchen paper towels and pushing them into a funnel stem can eliminate virtually all particles, the filtration is slow, however, but faster than sequestering in the refrigerator (allowing the fine particles to settle).
10.
Pyrex Measuring Jug - this is helpful with filtration and removing extract from broad containers (such as cooking pots) as well as measuring solvents for extraction and washing.
11.
Drying Dish - The dish should be deep enough to accommodate the amount of solvent used. Ceramic plates can be used too, ones with gentle curving edges and plain white glaze are quite good for being easy to scrape, though they can only have about 100ml in them.Several such plates would be necessary for an extraction - this can be a good thing for seeing what each consecutive pass gets out.
12.
Scraper Blades - These are essential for scraping up the final product, the best ones are the single sided ones used for removing stickers from glass. They have the advantage of being easy to handle and able to bend slightly for getting around corners in drying dishes.
13.
Acid - I recommend tartaric acid, which can be bought from supermarkets from the cakes and lollies section. Other acids can be used, but hydrochloric acid, in particular, should only be used with fully intact enamel pots or with pyrex pots.
Tartaric acid is handy because it only takes a teaspoon to turn 10L of water to around pH 3-4. Citric, acetic, and ascorbic acids can be used too, though beware of acetic acid if DCM is used in nonpolar washing as the acetate salts of DMT are fairly soluble in DCM.
14.
Base - Sodium Hydroxide (NaOH - often sold as drain cleaner, but be sure that the drain cleaner you get says '99% sodium hydroxide', it is also known as 'caustic soda' and in the US the brand Red Devil Lye is allegedly good - in fact anything called 'lye' is a base, but traditionally it was potassium hydroxide), Potassium Hydroxide (KOH, sold at hydroponic shops as pH up, and used to make liquid soaps).
NaOH and KOH are both strong bases and should be dissolved 1:10 at least before using (premixed solutions from the hydro shop are fine as is). Some suggest using ammonia, but domestic sources of it are not as clean as NaOH, thus I do not recommend it.
Always add sodium hydroxide and potassium hydroxide to water, and not the other way around. When working with strongly alkaline solutions it is recommended to wear safety glasses and gloves. Read my warning for more information
15.
Washing Soda - Sodium carbonate is usually available from supermarkets sold as 'water softener' - the way it works is that it increases the amount of sodium in the water which helps bias the ion levels in water in favour of sodium, as opposed to calcium, magnesium and iron, which have substitution reactions with the sodium-fatty acid salts in soaps which reduces their frothing and can produce an insoluble precipitate (calcium and magnesium-fatty acid salts mostly).
16.
Non polar Wash Solvent - Toluene (commonly used as an octane booster, also used to dissolve vinyl glues, for laying vinyl flooring), and xylene (available in many hardware stores, I have heard of it being used to remove the resins that are used to coat tiles - presumably urethanes). The aromatic solvent is used in this technique because it dissolves a lot of stuff, in the defatting stage, where a solvent which clears a lot of gunk is useful.
I recommend turpentine for the simple reason it is much easier to get, much cheaper, does the job just as well, and is less toxic. It is possible to use high boiling naptha (sold as 'white spirits' in australia ) and some have suggested the use of parrafin wax which is able to be easily separated as it sets hard when cooled.
17.
Extraction Solvent - There is basically three choices for this, and which one used determines how one must do the separations. Ethyl ether (from automotive stores as starter spray) and methylene chloride (also known as dichloromethane, or DCM) both share the property of having a very low boiling point (around 40°C) and consequently, when using them at room temperature, using a turkey baster, sucking up these solvents will be an exercise in frustration, one definitely needs a separatory funnel, and strict procedure of venting when agitating.
The solvents evolve a lot of gas, often at higher than ambient air pressure, so they pump themselves straight back out. Thus if a turkey baster is used and the Non polar is one of these, one must remove the polar phase, as this will not cause the same problem. With DCM this means pulling the top layer (DCM sinks) and ether, pulling the bottom layer.
A separatory funnel makes the use of DCM much more enjoyable, since the tap is at the bottom and that's where the DCM ends up too. DCM also absorbs a lot of the desirables very quickly. Naptha (aka shellite) is readily available, and is easy to work with using a baster.
If one looks around, there are other good options too - hexane fraction, which can be found for a pretty good price is available, and hexane has about 2-3x the solvation power of shellite/naptha.
Be very careful with shellite/naptha and ether, they are highly volatile and explosive. Read my warning for more information. Dichloromethane can damage the lungs, care should be taken when using it too.
18.
Recrystallising Dish - From limited experience, it seems that the best container for this is a dish which has a curved inner surface (like a noodle bowl), and plastic wrap is used to prevent the solvent from rapidly escaping.
Scraper blades will probably need to be bent into a curve to scrape the edges properly, though a scalpel might serve better for removing the crystals. A double layer of plastic wrap is good for ensuring that it doesn't stretch down too much when it cools (the gas trapped inside will contract when it cools). You don't want the naptha venting into your refrigerator, it smells bad.
19.
Recrystallising Solvent - Due to it's higher boiling point than any other available, and it's fairly reliable homogeneity, if possible, the best solvent is isopropyl alcohol (IPA). Naptha will also work, though the lower the boiling point of the solvent, the more it will evaporate away while handling, which can be a pain.
Acetone can probably be used, as can methanol and ethanol. Ethanol seems to need very little to dissolve the material, which can be problematic with very small quantities (a gram or less). Slightly polar solvents are good in this step as tannins dissolve quite well in them, if they get to the final product.
Acetone and ethanol have not been tested as far as I know, but I do know that acetone dissolves DMT freebase quite well. With all but naptha, it is essential to save already formed crystals to seed the solvent once it has been cooled.
20.
Dropper Bottle - This is used to transfer the hot recrystallisation solvent into the recrystallisation dish (specifically, the dropper)
21.
Nitrile/Neoprene Gloves - most domestic glove manufacturers now sell a special kind of glove for people who are allergic to latex (IMHO latex is nasty anyway), there are two types, neoprene and nitrile, the former are thicker and are particularly good for handling hot liquids, the latter are good for handling Non polar solvents, particularly aromatics which will very rapidly decompose latex.
I have come to the conclusion that it is crazy to work with these materials without using good protective gloves. In particular when agitating washes and extractions involving highly volatile solvents (ether, dcm, naptha) this permits venting of jars without exposure to the solvents. One will get tired of having dried out skin from the base liquid that inevitably ends up on one's hands during the process too.
22.
Safety Glasses - This is recommended for any stage involving the use of sodium hydroxide, and to a lesser degree, non polar solvents, as protection against damage to the eyes that can occur. In particular, sodium and potassium hydroxide can burn the eyes and even blind you if they damage the eyes enough.
It is most important that if one is using hot naptha that you vent regularly, otherwise you could end up with a small explosion (not flames, just from vapour pressure) of pH 12.5-13 solution in your face and all over the room.
Step 1 - Prepare the Bark
The bark must be prepared for extraction, a simple but effective method that can be used is to simply pull strips of fibres off using fingernails (or assisted with a pocket knife) so that thin pieces are removed - this must be done when it is still fresh.
The bark can be cut up into small pieces and put through a blender or coffee grinder, this is best done when dry, though cutting it up when dry can be difficult, it would be best done when still fresh (it is best to ensure cutting goes from the inside of the bark to the outside because the inner fibres are long and resistant to being cut).
If bulk quantities are being worked with (like 10kg or more) a mulcher can be very effective. A small garden shredder is very helpful in any case, and for anyone intending to powderise the material, it needs to be broken into small pieces before putting into a blender.
The more the bark is munched up the faster and more thorough first two steps are.
Step 2 - Acidification and Aqueous Extraction
This step uses an acid to make the tryptamine alkaloids soluble in water - the acids ionically bond weakly to the amine tail of the tryptamines and render them soluble in water like any other salt. This permits other elements in the solution which are less soluble in water and sparingly soluble in water to be removed in the next step.
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Prepare a solution of water with the pH adjusted to 3-4 with the acid you are using. |
When doing this, there is no reason to use distilled water. In fact distilled water may present a greater degree of trouble with emulsions later on. Hard tap water is probably in actual fact better, and by the time it is to be extracted it has been concentrated by a factor of 3-4x, via the reduction, it will have significant amounts of calcium and magnesium salts which react with surfactants (which cause emulsions) substituting for the sodium or (much more rare) potassium in the surfactant agent (which is usually a soap-like substance) and making a grey precipitate. Detergents are much more resistant to this but the surfactant action is significantly diminished. |
Add to the plant material to the solution, either soak (a couple of hours for powdered material, overnight or longer for less finely shredded material) or simmer for 1 hour. |
One can adjust the pH after adding the plant material, it often rises a little as some of the sap of the plant starts to get into the water. It is not a big deal though. |
Pour off the liquid and repeat two more times with more acidified water. |
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Filter the solution with progressively finer filtration devices (using progressively finer filters makes the process much faster). The best sequence is colendar, coarse strainer, tea strainer, coffee filters and then tissue paper plug in a funnel. |
Rather than using the tissue paper filter it can be substituted with cooling the solution in the fridge until all the fine particles settle and then decanting the clear liquid. There is little difference in time required for either method, although the filter plug is guaranteed to leave virtually no fine particles. Actually, the tissue plug filter is definitely faster. |
Combine the extractions and reduce on gentle heat until you clearly see that the solution is getting a skin of insoluble material. Filter the material again to remove the gunk that will precipitate out of this to some degree. |
I have changed this to 'a skin of insoluble material' because that's generally what I have done most of the time. The less bulk you have to work with, the better it all works. Be careful when it gets to this point because the temperature starts to go up as the solution's boiling point rises at about this point. |
Step 3 - Non polar Wash (Defatting)
This step uses the fact that the alkaloids are now well dissolved in water to permit the use of an aromatic solvent (which would readily dissolve the alkaloids in freebase form but not as the salt) to thoroughly strip anything from the solution which will contaminate the product at the end of the process. There is significant likelihood that the bark contains small amounts of histamines, which will be removed by this as well; in susceptible persons, histamines will cause the throat to constrict and make breathing difficult when smoking the product, which is an unpleasant side effect that is best avoided. This also removes any turpene type compounds which are usually present to some degree in bark, and will also go some way to reducing the tannins and fatty alcohols which will probably be present. Aromatic solvents are suggested in this step because they dissolve more than any other Non polar solvent, and thus clean the product more than ether, chlorinated solvents or naptha/shellite. |
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Pour the acidic extract into the separating container (separatory funnel or jar). |
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About 100ml of the aromatic solvent (toluene or xylene, or at a pinch, 200ml of naptha) is added and the jar is gently agitated (swirling, stirring, end-over-end). The quantity of solvent used should be about 10% volume of the aqueous phase, a little less for toluene/xylene, a little more for naptha. |
Aromatic solvents are used in this step because they have high solvation power, and will remove anything that might contaminate the final product much more effectively than non-aromatics (aliphatic is the technical term). Adjust the volumes of solvent upwards in the case of lesser solvents (such as naptha) to ensure it pulls as much of the gack as possible, also use more solvents if one is working with a larger quantity of material. If you got your solvent in a tin, no matter how delicately you agitate it, you will probably get a stubborn emulsion. I believe that adding a small amount of something which reduces the frothing effect of detergents and the like, such as calcium chloride (used in dessicating things like damp-rid and dri-rite etc). |
Separate the aqueous phase from the aromatic solvent phase. |
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Repeat the wash with the aromatic solvent two more times. |
The reason for doing more non polar washes is that the primary contaminants in the product is usually from not doing sufficient washes at this stage. In the case of toluene, 3 passes does the job quite nicely. If naptha/shellite is used, 4 or 5 passes may be needed. |
Do a final wash using the solvent that will be used for extraction to remove any excess aromatics suspended in the solution. Not neccessary if one used naptha as the defatting solvent. |
This is done to eliminate the majority of the high boiling aromatic solvent from the solution so when it is extracted the high boiling component of the solvent is reduced. If there is materials that boil at a significantly higher temperature than that of the DMT (i.e. much more than 120°C) the DMT will not crystallise or dry properly, as it will boil before the solvent it is mixed with. This is known as 'oiling out' and is best avoided if possible. |
Step 4 - Basify to pH 13
In this step the pH of the now washed extract solution is raised to 13, which will drive the alkaloids out of the water by binding up the acids that caused the alkaloids to be water soluble. |
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Mix up a solution of the base - for sodium hydroxide, 5 teaspoons to 250ml is sufficiently dilute. |
If one is concerned about pH spikes from introducing a solution this concentrated, twice as much water can be used. The pH of the solution made via the instructions to the left is around 13.5 or so, and really it isn't too strong. The main thing is adding it slowly while stirring. In actual fact, the only way that strong base could cause a reaction which destroys ones product is by adding it dry to the acidic extract solution, which could produce small local temperature spikes surrounding the beads of hydroxide and this could destroy alkaloids for sure. |
Add the alkaline solution slowly to the acidic extract, after adding it to the separating container, stir well while adding the base. Stop the process when the pH gets to around 12.5-13 |
There are many ways to do this, some people use a baster to transfer the solution, and use it to stir and pump the solution around, it can also be added slowly by pouring it in while stirring with a skewer. I don't recommend basifying in one container and then transferring to another. The DMT can stick to a lot of plastic and glass surfaces, and ideally one wants to get as much of it as possible. |
Step 5 - Non polar Extraction
Making the pH to 13 drives the tryptamines back into freebase form, in which they are insoluble in water. They are, however soluble in Non polar solvents, such as the ones described as suitable extraction solvents (ethyl ether, DCM and shellite/naptha). This property permits the separation of the freebase from the basified aqueous extract solution. Using a pH this high also eliminates emulsions.
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Add a quantity (100ml is a good amount for an extraction with an expected yield under 3g) of the extraction solvent to the basified solution. |
The amount of solvent to use depends a lot on how much you expect to get from the plant material. As a rule of thumb, 100ml of naptha/shellite will dissolve about 1g of DMT, less is needed for dichloromethane and ether, about 50-70% of the volume used for naptha in general, though the amounts must be kept practical for the separation method being used. Also note that using an excess of solvent may result in more being extracted than desired. This is particularly the case with naptha. |
Close the container, gently agitate, periodically vent to release pressure |
Some guides recommend heating the extraction solution to increase how much it draws across when doing this, I must stress that this will dramatically increase the amount of pressure that will be generated by the agitation. Having almost lost my vision from not venting a jar of hot shellite and having the jar pop and spray everywhere, I don't recommend heating the solution at all. Some guides say 'keep the base cool and the solvent warm' - this is not physically possible, the heat in the total solution will very rapidly equalise, especially if it is shaken vigorously. When venting, you will find that pressure builds up more initially, and venting should be frequent at the beginning of the agitation process, but you will find that after a doing it a few times that the pressure buildup is much less and at a certain point you can just keep shaking it because it does not build up further pressure. |
Separate the nonpolar solvent from the basified solution. Repeat this 3 times with an identical amount of nonpolar solvent. |
Because the pH is high, at around 13, and because the solution has been thoroughly washed, it will not form stubborn emulsions, the differentiation of the layers usually is almost perfect within 5 minutes. I have subsequently worked out that the use of 'hard' water helps a lot with ensuring you get no emulsions, and possibly the addition of a small amount of calcium chloride or magnesium sulphate (I think the former is better) can harden the water and reduce its capacity for frothing. It is not neccessary to wait long - 5 minutes of gentle agitation and 10 minutes of settling is usually long enough for each pass |
Step 6 - Polar Wash
This step is done to eliminate any residual polar soluble contaminants present in the Non polar extraction. The main concern is the base itself (which burns hot and makes the product harsh), though there is also problems involving contamination from the aqueous fraction also, plant substances etc. Generally speaking the stuff washed in this step will not prevent crystallisation if left in, but it should not be left in because it is just yucky. |
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Add an amount, about maybe 5% of the volume of nonpolar, of water adjusted to a pH of at least 10 with sodium carbonate to the non polar extract solution. |
The best way to do this is to add an amount of sodium carbonate (washing soda, available in the detergents section as a 'water softening agent), just enough to the degree one finds the solution makes one's fingers slippery when dipped in it, and then add more water until the sliming effect stops (This should result in about pH 10 or so) |
Agitate the mixture gently for about 5 minutes, let it settle before proceeding |
Gentle agitation is essential to ensure that no microdroplets of alkaline wash water remain in the nonpolar extract solution. If more violent agitation is used, expect to wait a lot longer to ensure that all the microdroplets of the alkaline wash water are completely separated. |
Remove the water from the nonpolar extract, and repeat this wash two more times. |
Repeating the wash three times will ensure that none of the base or other polar soluble undesirables remain in the solution. This step is critical for removing residual hydroxides and salts of the acid and base being used. If this step is not done properly, the hydroxides will react with the freebase and destroy them, not to mention burning the throat. |
Wash one last time with a very small amount of tap water. |
This final wash is to ensure that the salts that might be hanging around are significantly diminished in quantity. Use only a very small (5-10ml) amount of water, not much is needed to ensure that you eliminate any residual sodium hydroxide and carbonate. |
Step 7- Evaporate Non polar Extract
Next, put the combined Non polar extracts onto a drying dish, something that will permit the easy scraping of the materials.
Using an electric fan to blow the drying dish vigorously is a good idea, it dramatically increases the rate at which the solvent evaporates off.
Do not do the evaporation in a poorly ventilated space, doing so risks possibly starting a fire if a stray spark occurs in an adequately concentrated region of air containing the vapours.
Although it probably helps with getting all of the extract out of the dish, it is not absolutely necessary to bring it fully to crystallisation at this stage. This will take at least 12 hours to fully happen under a fan. The extract is easier to remove from the drying dish if it is fully dry as it has a much harder consistency and comes free of the glass much more readily. One may be able to ease the removal of the product if it is in a gooey state by putting the dish in the freezer for half an hour, covered in plastic to ensure no water condenses onto it.
Step 8 - Recrystallisation Purification
This step is done to refine the product further, and indeed can fully purify the extract to translucent crystals. The longer this stage is done, the larger the crystals can become. When recrystallising, the idea is to use a solvent which dissolves undesirable elements better than the desirable element, hence with study, the best possible solvent or mixture of solvents can be developed to clean the product most effectively. This step eliminates contaminants in the product which will make it harder to smoke. |
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Heat the recrystallisation solvent until it starts to boil by sitting in a container over water heated in a jug. |
A good container to put the recrystallisation solvent in is one which has a dropper in it, as you can simply let it sit in the water until it gets to the same temperature as the water, and then you can immediately drop the solvent onto the freebase. Keep the lid on the dropper bottle of the solvent loose so any pressure from the boiling does not build up. |
Place the scraped up product from the previous step into the recrystallisation container and allow the container to get nice and warm. |
Be careful here not to let the freebase get so hot that it boils, as this will cause a loss of product |
Slowly add the hot solvent to the warmed recrystallisation container, stirring and agitating until all of the product is *just* dissolved. Be patient with this, mix it until it is clear that no more mixing will increase dissolution. |
The idea here is that the minimum amount of solvent, at the highest temperature possible (at which it will dissolve the most possible product for the volume), which, when cooled will not dissolve the product very well at all, and thus it will precipitate as crystals. |
Seal the recrystallisation container. |
A jar can be used for recrystallisation - when the product crystallises hard as it does in this process, it can be scraped out using a scalpel or a piece of wire. If using a beaker or bowl, a double layer of plastic wrap is recommended, and fixed in place using a rubber band. Sealing the container simply prevents the crystallisation of water when the container is put in the freezer. |
Let the container cool to room temperature. |
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Optional: Alternate between the fridge and outside the fridge every hour or so for as long as you like. |
The colder temperature causes crystals to precipitate, and then warming them again dissolves the smaller crystals more rapidly than the larger crystals. When done for long enough, this favours the formation of large homogenous (containing only one substance) crystals. In the case of acacia obtusifolia, there is only DMT and NMT. The NMT forms an amorphous yellow resin, and with the correct choice of recrystallisation solvent, can be selectively removed, leaving behind only the DMT, which is a translucent waxy crystalline substance. The DMT, in any case, (and I think this applies to 5 methoxy DMT) is a clear crystal, the yellow or brown or red colour common in extracts is not from the DMT. It improves the resulting size of the crystals if the initial room temperature/refrigerator stage is done for a lot longer, this causes the crystal cores to trap less contaminants. |
Optional: Then alternate between the freezer and the fridge for another period of time. |
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While still at freezer temperature, discard the solvent (it has very little in it of value - you can verify this for yourself by evaporating and inspecting it). |
Because the extract was just dissolved at close to it's boiling point, at the temperature in a freezer there is a very insignificant amount of the desirable alkaloids remaining in solution. With the right choice of solvent, the DMT can be preferentially precipitated and thus isolated from the other components in the extract. You may find that a yellow gummy substance has aggregated at the centre of the container, this can be persuaded to come out more readily with a few drops of water. It is tannins, and they absorb a lot of water, and doing so will make them more readily sensible to pouring out past the crystals, which generally will be firmly attached to the sides of the container. |
Repeat up to two more times, using denatured ethanol or isopropyl alcohol (99% isopropyl) keeping several of the formed crystals from the first naptha recrystallisation aside to add to the recrystallisation container one you see that an inchoate precipitate has formed, and this will 'seed' the growth of the crystals from the precipitate. Keep it in the freezer during the whole process. |
If done more times, the extract is much cleaner. Using alcohol in subsequent recrystallisations greatly eliminates problems from tannins and hydroxides, as they are much more soluble in the alcohol than the DMT, especially because of the presence of a small amount of water in the alcohols. The crystals that form from naptha are often cubic, indicating that they are partially formed from sodium salts, but from alcohol they form crystals more resembling quartz with hexagonal cross-sections and points. |
Dry the final recrystallisation. |
When the extract is very pure, the product will be very easy to remove from the container. A scalpel is a good device for this, one with a curved blade. |
Conclusion
I have written this extraction procedure in the hope that others who find the lack of clarity and good chemistry information in most guides offputting, also this guide exposes a number of myths regarding times required for processes, in particular the Non polar extraction.
The product resulting from following this guide, assuming one begins with a good source, should be just about as pure as the product can be made. Also, if a neophyte follows this process, and they have started with good material (good material is equally important as the right technique, you can't get gold out of you put garbage in), it is almost guaranteed one will get a good result.
I will be revising this process until it becomes clear that it covers the topic in a thorough and concise way, it is my hope that this document will ease the transition from neophyte to journeyman that can be extremely frustrating and drawn out. Accurate information will ensure that so long as the directions are followed, good results will come out at the end.
Reports of using this guide will be appended to the end, I encourage anyone who has had success with this technique to send me their reports so I can add this to this document to demonstrate the efficacy of the technique, and to encourage neophytes to keep trying if they do not do as well as they expected.
One final comment, most people will not get as much as they hope for out of extractions. Over a process of a number of extractions one gets a better idea of how much to expect, the visual appearance of quantities of freebase of various weights will take a while to know, as will the amounts of plant material that produces it, and in some cases, the right times and ways to collect the material will also influence the results. Do not be disheartened if yields are lower than you expect, only experience will teach you how much to expect in practice.
Appendix
I decided it would be a good idea to add an appendix to briefly discuss some other modifications to the process which have had limited testing done on them.
Dry Acid/Base Extraction
As yet, the only method tested so far on this method has been to do an acidic aqueous extract and then dry the material until it is hard and dry over a steam bath (in cooking, this is called a double boiler), however this method is less than satisfactory as it risks degrading the alkaloids. The defatting is done on the dry material directly, and a significantly greater degree of effectiveness of both defatting and extraction has been observed.
Another option for dry acid/base extraction which has not been tested yet is to make sodium ethoxide (sodium ethylate) and basify it 'dry' this way. This could be done as follows:
1.
Dry and grind plant material into fine powder
2.
Add the ethanol to the plant material until it forms a paste and add about 1 teaspoon of a dry solid organic acid, such as citric, tartaric or ascorbic acid, and then mix them through thoroughly (I just tested to see if tartaric acid dissolves adequately in ethanol, and indeed it does) this step is to 'dry acidify' so that 'dry defatting' does not get any of the goodies.
3.
Dry the acidified bark powder out, a simple steam bath is a good way to ensure it is fully evaporated (this is like a double boiler, sitting the container atop another container with water boiling underneath. Having a fan blowing past it is probably both safer and faster for this.
4.
Place the powder into a jar or bottle, and soak the acidified bark powder in toluene, just cover the material, shake it up and let it absorb for about an hour, and repeat this process, decanting off the liquid until the solvent that is poured off does not acquire any colour or clouding.
5.
Allow the plant material to evaporate off all of the solvent, the same way as the excess ethanol was removed from the dry acidification.
6.
Make up a solution of sodium ethoxide (add sodium hydroxide to denatured ethanol, mix it up, and stop adding more sodium hydroxide when it clearly is not dissolving any more into the alcohol), and turn the defatted powdered plant material into a paste mixing it thoroughly.
Again, dry it out over as steam bath with a fan to blow the vapours away from the heat source. After doing this, the DMT is fully basified and now will readily transfer into a nonpolar solvent.
7.
Get your extraction solvent (naptha/shellite, hexane) and add it to the powder, in a jar or bottle again, just until it covers it. After giving it periodic shaking over the period of an hour, decant the liquid off, collecting it. Repeat three times.
8.
Filter the collected nonpolar solvent through a tissue paper scroll filter plugged funnel.
9.
Wash the nonpolar solvent 2x with sodium carbonate solution (basified just enough to the point before you start to get the slimy fingers effect from it) and one last time with a small amount of plain tap water. 5% of total volume of water compared to nonpolar is more than enough for the polar washes.
Although there is likely to be very little hydroxides because all water was eliminated in the dry basification, it is still good to ensure that nothing polar gets across floating around suspended in the nonpolar.
10.
Evaporate the nonpolar solvent under a fan in a well ventilated space to yield the crude extract.
This method should, theoretically, be more effective and efficient, and time efficient than stardard liquid/liquid extraction because, basically, water takes ages to evaporate, and solids dissolve into liquids at a rate much higher than partitioning between phases.
In fact, usually one gets 100% dissolution, further passes are simply to get it out of the liquid retained in the plant material. Being able to press the mass of plant material in between extraction passes would perhaps be equally effective, and use a lot less solvent, possibly only one step would be required then.
This method would probably work better (using less solvents) if one were able to press the sap out of fresh bark in the first instance, or something like that, but would require some pretty sturdy equipment to do it. In the methods of making virola snuffs, the natives take the fresh material and heat it over flame until the sap starts to ooze out and they collect the exudate.
This only really would works well if it is done immediately after taking it off the trees in situ, as the more the bark dries the less effective the use of the heat to make the inner contents exude the sap works.
