Version 0.2
Last modified: 19 April 2003
Copyright © 2003 Soma
This document is licensed for redistribution under the GNU Free Documentation Licence
When modifications are made, put credits below this line.
WARNING (READ THIS FIRST)
Acknowledgements
Introduction
The
Plant
Equipment
and Chemicals
Step
1 - Prepare the Bark
Step
2 - Acidic Extraction
Step
3 - Nonpolar Wash (Defatting)
Step
4 - Basify to pH 13
Step
5 - Nonpolar Extraction
Step
6 - Polar Wash
Step
7 - Evaporate Nonpolar Extraction
Step
8 - Recrystallisation Purification
Conclusion
Extraction
Reports
Changelog
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).
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) have been taken less than 24 hours beforehand, the
same goes for beer and wines, and there are foods which contain proteins which
are very 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.
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 protein 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
bloodpressure 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 nonpolar solvents (turpentine and naptha/shellite) 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), there
is also neoprene gloves available, but these will be easily distinguished by
being thicker and 'insulating' will be mentioned on the packaging somewhere.
Nitrile is the best to use as it is highly resistant to turpentine and
shellite.
Turpentine is not so bad, and being such a high boiling material,
it's vapours are unlikely to develop to an extent to cause breathing problems.
However, shellite is very volatile, more volatile than petrol, and probably
more explosive than petrol.
No sources of flame or sparks should be present when
working with shellite, 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.
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
ventlation 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 .
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),
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), Glorfindel (for his excellent points
confirming the pH 6 idea and pointing out the need for pH 12.5 or higher for
polar washing), Gumby, for emphasising the safety factors, and anyone else who
I have gathered information regarding this process who I might have forgotten.
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.
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 6, 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 unneccesary so long as the base is
diluted). The acidic solution dissolves less undesirables when the pH is only
lowered to 6 (which is not very much, but this is the pH at which 99% of the
DMT stays in the water), and there is no problems at all with emulsions with
the pH above 12.5. Washing should also be done at this high pH, since it has
been pointed out that for washing one should not use a solution which will
ionise the freebase at all.
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
neccessary time stated), when in fact the best results seem to be from doing a
nonpolar wash of the acidic extract and using a fairly low pH (like 8-9) and no
salt, for washing the nonpolar extract. Washes ensure the resulting product is
as free from contaminants of a non-alkaloidal nature as possible.
And 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, which is known variously as 'naptha' or 'shellite',
the latter being the most readily available solvent for use in australia.
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.
I will also focus on the equipment which will ensure the best results with
the least outlay without any compromise of effiacy of the process.
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.
The gobbledygook jargon of botanists really works well for those who
understand it, but the rest of us are overwhelmed and frightened by it, so some
good info in identifying it is needed. There are numerous efforts being made at
cultivating this tree so that harvesting of wild materials becomes completely unneccessary
except for botanical and analytical purposes, however at the moment, it looks
to be five to ten years before any of these efforts become viable sources. The
plant is quite prolific, and I believe that it is unlikely to face extinction
before it can be sustainably produced.
The guide should be applicable to other sources of DMT, as the method
described is very thorough.
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.
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.
The more the bark is munched up the faster and more thorough the next step
is.
|
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. |
|
|
Prepare a solution of water with the pH
adjusted to 6 with the acid you are using. |
For this step, I recommend using vinegar, as it will not concentrate
when boiled down. Acetic acid boils at 117°C, and though it is hygroscopic, it does not
hold as much water to it as hydrochloric acid, which will stay in solution
until ~38%, thus reducing it will concentrate it. The pH of 6 is used because this is the highest pH that will ionise
the DMT, and because it is not so low as conventional techniques use, it will
not dissolve anything with a pKa lower than DMT. |
|
Put the bark in the pot and add the acidic
solution until it just covers the bark. |
|
|
Bring the pot to the boil and then turn down
just to the point where it is not bubbling. |
|
|
Gently simmer for 1-2 hours. |
The exact length of time required depends on how finely shredded the bark
is, fine powder has been shown to extract very rapidly simply by using hot
acidic water. If the material is coarsely shredded, it needs longer to fully penetrate
the fibres. |
|
Up to two more quantities of acidic water
can be used to extract the remainder of the alkaloids, follow the last four
steps the same way as the first. |
Experiments seem to show that on average, between 60 and 80% of alkaloids
migrate across in the first acidic extraction. This is probably also related
to how finely the material is ground as well, and how long it is cooked or
soaked. It is a good idea to do at least a second pass, and the large majority of
alkaloids are completely extracted by doing three passes. |
|
Run the material first through a coleander
and then through a coarse strainer and discard the plant material after the
three extractions are done. |
|
|
Reduce the volume of solution to whatever is
practical for the container that will be used for defatting and extraction. |
If highly powdered materials are used, a lot less liquid is needed to
extract the alkaloids. In some cases no reduction is required at all, I have read reports of
powdered mimosa hostilis root bark being of such a small volume that reducing
was completely unneccesary |
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Run the reduced extract through the
felt/fluff filter to get the bulk of the crud out. Press it to remove the
liquid it retains. |
|
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Run the reduced extract through a
tea-strainer to catch all the medium sized particles |
|
|
Finally, filter the reduced liquid through
coffee filters. |
I recommend this filtering regime because
particles in the acidic solution can interfere and make emulsions worse, as
well as introduce elements of the defatting solvent and what it dissolves
into the extraction phase. |
|
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 likelyhood 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. Aromatic solvents are suggested in this step because they dissolve more
than any other nonpolar solvent, and thus clean the product more than ether,
chlorinated solvents or naptha/shellite. |
|
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Pour the acidic extraction into the
separating container (separatory funnel or jar). |
|
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About 100ml of the aromatic solvent (turps,
toluene or xylene) is added and the jar closed and shaken vigourously. |
Aromatic solvents are used in this step because they have high solvation
power, and will remove anything that might contaminate the final product. I recommend turpentine because it is cheap, does the job, and isn't as
nasty as toluene and xylene. In actual fact, the solvent that will be used for extraction can be used here,
but usually the extraction solvent is more expensive than any given aromatic
solvent, and may not be as effective at washing than aromatics. |
|
Separate the aqueous phase from the aromatic
solvent phase. |
When doing this separation, it is not neccessary to wait as long as many
guides recommend. It is well separated within half an hour and if let to sit
overnight will form a gel-like consistency. Do not be concerned by the seeming lack of separation, more time will not
clarify the aromatic wash layer. The best way to do the separation with a turkey baster is to draw off the
lower layer, this enables you to avoid bringing across the solvent as much as
possible, and it is much easier when using a turkey baster to get a full
separation as when you get down to the bottom you can tilt the jar or
container sideways and maximise the height of the aqueous layer, making it
easier to cleanly separate. If one is concerned about losing aquesous solution by discarding the
emulsion/wash, simply collect the washes in a jar and let them settle,
usually a small amount of the aqueous extract will resolve further, about 10%
of the volume of the total wash solvent volume at the most. |
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Repeat the wash with the aromatic solvent two more times. |
The reason for doing more nonpolar washes is that the primary contaminant
in the product is usually from not doing sufficient washes at this stage. |
|
Do a final wash using the solvent that will be used for extraction to
remove any excess aromatics suspended in the solution. |
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 (ie much more than 65°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. |
|
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. |
|
|
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. |
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Add the alkaline solution slowly to the
acidic extract, stir well while adding the base. |
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. |
|
Making the pH to 13 drives the tryptamines back into freebase form, in which
they are insoluble in water. They are, however soluble in nonpolar 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. |
|
|
Add a quantity (100ml is a good amount) 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, 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 shellite. |
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Close the container and shake it
vigourously, venting between shaking to release pressure buildup in the jar. |
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 explode, I don't recommend heating the solution at
all. Note that when venting, the amount of pressure buildup will reduce the
more emulsified the solution becomes, at a certain point no more venting will
be apparent and at this point shake the buggery out of it. The more
thoroughly it is shaken, the better it extracts. |
|
Let the emulsion settle, then separate from
the basified solution. |
Because the pH is high, at 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 |
|
This step is done to eliminate any residual polar soluble contaminants
present in the nonpolar 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 excess of water adjusted to a pH of at least 12.5 to the nonpolar
extract solution. |
With this step, the more water the better, as more water will more readily
remove undesirables. The high pH used is to ensure that the water does not ionise the DMT and
make it water soluble. |
|
Close the container and shake it vigourously, venting between shaking to
release pressure buildup in the jar. |
Refer to the notes above about venting. When using low boiling solvents
such as the extraction solvent, shaking causes pressure buildup, and not
venting can lead to a popped lid and loss of product (and in the previous
step, possible loss of vision). Vent until no more pressure builds up from
further shaking, then shake vigourously. |
|
Let the emulsion settle, then separate, and repeat this wash two more
times. |
Repeating the wash three times will ensure
that none of the base or other undesirables remain in the solution. |
Next, put the combined nonpolar extracts onto a drying dish, something that
will permit the easy scraping of the materials.
Using an electric fan to blow the drying dish vigourously is a good idea, it
dramatically increases the rate at which the solvent evaporates off.
If the proper equipment were available, a drying dish that uses vacuum would
be even faster, and would permit recovery of the solvent, though this is not
accessible to most people who wish to do this process.
Although it probably helps with getting all of the extract out of the dish,
it is not absolutely neccessary 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.
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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 tothe same temperature as the
water, and then you can immediately drop the solvent onto the freebase. |
|
Place the scraped up product from the previous step into the
recrystallisation container and allow the container to get nice and hot.. |
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 the warmed
recrystallisation container, stirring and agitating untill all of the product
is *just* dissolved. |
The idea here is that the minimum amount of
solvent, at the highest temperature possible (at which it will dissolve the
most possible product), which, when cooled will not dissolve the product 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. |
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Let the container cool to room temperature. |
|
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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 obtusifola,
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. |
|
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). |
Because the extract was just dissolved, 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. |
|
Repeat up to two more times |
If done more times, the extract is much cleaner. |
|
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. |
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 nonpolar 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), is guaranteed to 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 effiacy 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 amouts 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
practise.
soma
email me:
soma8@eml.cc
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Need I say it, all of these reports are from people who have done these
processes where doing so is legal, and all are anonymously sent to me to add
here. |
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Mimosa Hostilis Extraction (13 April 2003) Materials; A few 500ml flasks/beakers, a jar, seperatory funnels, vacuum
hand pump, glass funnels, I started by boiling 325ml of distilled water, then took it out of the pan
and into a beaker where I acidified to a PH of about 3 or 4 using muriatic
acid. Then I poured this acidic water in a jar containing 88.4 grams of finely
powdered mimosa hostilis root bark. Since I used hydrochloric acid I decided
not to add all three acidic water extracts together and reduce volume because
I didnt want to concentrate the acid. So what I did was each of the 3 extracts on there own. After puting the
acidic water with the root bark I waited 1 hour and pured the liquid/root
bark into a cheese cloth on a beeker, and sqweezed all of the water out. I
then took the dry root bark and put it back in the jar with the same amount
of acidic hot water as the first time. And while waiting another hour for that to finish up I filtered the liquid
from the first extract into a funnel with cotton and a vacuum pump connected
to the flask. Then I defatted by putting 80ml of xylene and throwing away the
xylene/emulsion. I defatted 2 more times with naptha(80ml). Then I basified with NaOH, when it was about half way threw I added some
naptha and kept basifying untill it turned a slippery black type color. Then
I seperated the naptha with the emulsion and added 80ml of warm naptha. I
seperated that naptha/emulsion and added another 80ml of warm naptha.
Again I seperated and kept the naptha/emulsion. Now I took the naptha/emulsion and added some PH 8 distilled water and
threw away the water. This got rid of most of the emulsion, I put the rest in
a graduated cylander to further seperate. I washed the naptha 2 more times
with PH 8 dH2O. I evaporated the naptha via fan and dish to reveal .4grams (400mg)of white
fliffy crystals. By this time the second soak of root bark was ready to be
further extracted so I put that through a cheese cloth and cotton funnel and
then put more acidic water with the root bark. I defatted this time with only naptha 3 times. Basified and extracted and
washed just as before. I evaporated this to find .22grams of crystals. I
extracted the last of the acidified water by filtering, defatting, basifying,
added naptha, washed naptha and evaporated just as before to get .06grams of
crystals. I did this whole extraction in under a day, and my yeild tells me I really
dont have to wait as long as some teks say. My total yeild was .68grams of
spice from 86.4g of mimosa root bark. That's .4grams the first one, .22 the
second and .06 the third one. As you can see the last extract is low but not completely insignificant.
If I were doing an extraction with a different acid like say acetic(vinegar)
acid I would have combined my extracts and boiled down to about half or 1/4th
it's original volume, but since I used HCl I decided it would be better to do
each seperately. |
12 April 2003
soma: First draft written
13 April 2003
soma: New instruction format implemented - using simple instructions on the
left and notes and clarifications on the right. This makes it a lot easier to
read. The recrystallisation technique was condensed to one step. Thanks to
mesqualero for the idea
14 April 2003
soma: Prettified the two column sections by making all the note columns grey
coloured, added a report, fixed the paragraphing. Thankyou to andrew for the
report.
15 April 2003
soma: modified polar wash directions to specify using water basified to at
least 12.5 after a suggestion from glorfindel from dmt world.
16 April 2003
soma: Added notes about doing further filtration.
19 April 2003
soma: Expanded filtration information, added a 'warning' section (thanks
gumby), added more equipment to the equipment section (strainers, filters and
safety glasses).