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methanol extraction,Yeilds wet crystal

crystal extraction methanol wet yeilds

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#1 Eskatari


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Posted 06 June 2010 - 04:08 PM

I recently extracted a brf cake that weighed 60 grams,50 mls methanol,2 and a half hours later, all over,boiled the cake in methanol for 40 mins,filter 4 times while hot,then evaporated the solution down until it starts to turn yellow ,And then i stuck the solution in the freezer as soon as it evaporated down low enough that the solution turned a lovely yellow colour.And at that stage u can see stuff slightly precipatating out,Stick it straight in the freezer,Psilocybin is more soluble in warm,45 degree temperatures than say 5 to 0 degrees and alchohol doesnt freeze,psilocybin becomes insoluble in alchohol that is at water freezing temperature,and also the alchohol will completely evaporate off in the ffreezer,there may be some water that didnt evaporate off left behind,but that will help form the crystals when there frozen,And both will disolve into liquid if taken out of the freezer for longer than 10 mins ,dissolves into a brigh yellow liquid,Smells like a beautiful mushroom liquer! not like my last batch whitch smell like ass and was orange and a small concentrated amount of orange-red-brown oil ,tasted like shit but seemed to work instantly when placed on tongue,it would dissolve into my tongue within seconds? hmm, I have yet to try this new batch,it looks alot more promising! nice yellow composure and what not. Has anybody else acheived this? im sure the crystalline product could be dried of water with dessicant or a fan ?:weedpoke:

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Edited by Eskatari, 06 June 2010 - 04:13 PM.

#2 koldj


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Posted 06 June 2010 - 05:06 PM

To my knowledge that stuff is just some sugars from the initial extract. The magic is probably decomposed and gone with the liquid... But there's a way to find out!! :D

#3 Eskatari


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Posted 06 June 2010 - 05:19 PM

it tasted really really mushroom like :D

#4 koldj


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Posted 06 June 2010 - 05:21 PM

Any effect yet?

#5 Swampy



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Posted 06 June 2010 - 07:18 PM

do the math. could that quantity of organic material possibly yield that quantity of crystalline psilocybin?

#6 Edzor


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Posted 06 June 2010 - 09:07 PM

try dissolving that stuff in ethanol and pop it in the freezer i think the good stuff will recrystallize and all the sugars n stuff will stay in solution http://en.wikipedia....ystallization

good luck

#7 Sidestreet



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Posted 07 June 2010 - 05:50 AM

Wouldn't the boiling kill the magic?

#8 Eskatari


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Posted 08 June 2010 - 04:58 AM

Yes it would if the temperature of the solution being heated goes above 48 degrees or reaches the point at which water boils under normal atmospheric pressure which is 100 degrees centigrade if i remember correctly,And methylated spirit (basically 95% ethanol,with approx 1.4% methanol and 3.6% water,Ethanol and water form an azeotrope when exposed to air to the point where it reaches 95%,so its quiet hard to obtain 100% ethanol,And uneeded for this) as i was saying,Methylated spirit boils at a lower temp than water (100) Ethanol boils at 75 degrees centigrade if i remember correctly,But when i did it i never went that high with the temp,I kept it at around 45 degrees for 40 mins initially when soaking/boiling/extracting the BRF cake,Then filtered and evaporated a bit one about 51 degrees.

Heat is alright, up to a certain point(above 55 degrees i reckon). Psilocybin breaks down when it's been in boiling water for too long too.

#9 whatchamacallit


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Posted 08 June 2010 - 06:03 AM

If you read the patent on extracting psilocybin, there is a lot of cleaning and stuff to get something that would crystallize. It involves much cleaning, different solvents, and column chromatography.

From here:

The active fungal material (fruit bodies, sclerotia and mycelium) is
carefully dried in an air current or under reduced pressure at 20-40
centigrade, finely ground and thoroughly extracted with a lower aliphatic
alcohol or with a mixture of water and a water-miscible organic solvent at
room temperature (20 to 30 centigrade). The extracts are concentrated under
reduced pressure at low temperature. The residue is defatted with petroleum
ether and extracted with acetone or chloroform-alcohol to remove inactive
accompanying material. Other ballast material is separated off by dissolving
the residue in as little water as possible and repeated precipitation with
absolute ethanol or acetone; the filtrate is concentrated under reduced
pressure at low temperature.

Further purification is advantageously carried out by chromatography on
cellulose powder in a through-flow process; elution is performed with water
saturated butanol or another alcohol not miscible with water. The fractions
collected are tested for their content of active substance by means of the
Keller reagent (glacial acetic acid containing iron chloride and
concentrated sulphuric acid). The fractions showing a positive colour
reaction are combined and, if necessary, chromatographed again on a column
of cellulose powder. From the through-flow chromatogram a rather rapidly
travelling zone is eluted.

This yields a product containing an active substance, "psilocin,"
characterized by a clear blue Keller reaction, while from a zone travelling
more slowly, a product containing a second active substance, "psilocybin,"
is obtained in larger amounts.

The active substances are obtained in a fairly pure state from the column
but contain halogen and do not crystallize out as Psilocybin and psilocin.
The halogen may be removed only by chemical treatment, crystalline compounds
being thereby obtained. For this purpose, an aqueous solution of the active
material is treated with silver carbonate or silver oxide. Excess silver
ions are removed with hydrogen sulphide and the remaining solution is
concentrated under reduced pressure at low temperature, the substances
crystallizing out from the concentrated solution.

For analysis, Psilocybin is recrystallized from methanol or water.
Recrystallization from water yields very fine white needles; from methanol
colourless hexagonal plates or prisms are produced; these contain methanol
and melt at 195-200 centigrade (with decomposition). The compound dissolves
in 120 parts by weight of boiling methanol or in 20 parts by weight of
boiling water; it dissolves difficulty in higher alcohols and other organic
solvents. The crystals are dried in a high vacuum at 100 centigrade, a
decrease in weight of 10.4% taking place. The results of elementary analysis
give the empirical formula C12H17O4N2P (molecular weight 284.2). Psilocybin
is an amphoteric compound. It is optically inactive and readily soluble in
dilute aqueous mineral acids and in dilute aqueous alkalis with which it
forms salts. A solution of Psilocybin in 80% (by weight) aqueous ethanol has
a faintly acid reaction (pH 5.2). The UV-spectrum in a methanolic solution
shows maxima at 222, 267 and 290 m~.

For analysis, the Psilocin is purified by another chromatographic operation
on a column of cellulose powder, using water-saturated butanol or by
treatment with potassium bi-carbonate in an aqueous solution and extraction
with ether or an organic solvent. The results of elementary analysis give
the empirical formula C12H16NO2. Psilocin crystallizes from methanol or
acetone; it is moderately soluble in water but dissolves readily in dilute
acid. M.P. 173-176 centigrade. (with decomposition). Psilocybin is the
phosphoric acid ester of Psilocin 4-hydroxy-dimethyl tryptamine
(Experientia, vol. 14, 1958, pages 397-399).

Psilocin is characterized by an UV-spectrum in a methanolic solution with
maxima at 222, 260, 267, 283 and 293 m~ and by the Keller colour reaction
which shows-unlike psilocybin-a clear blue colour.
The products of the present invention are psychotropically active and find
use in therapy as tranquillisers. Subcutaneous injection or oral
administration of 2 to 8 mg. of Psilocybin produces a pronounced euphoric
mood accompanied by a lack of spontaneity and a feeling of indifference.
When administered in higher dosage, there occur changes in perception
together with autonomic symptoms.

So please don't think you can use some alcohol to get pure psilo crystals. There has been loads and loads of debate on the crystals in alcohol. Many who've taken those crystals and separated them, and ate them didn't have anywhere the experience they would on that weight of psilocybin/psilocin.

The goodies will be suspended in the alcohol, and if evaporated, will dry to an unstable brown goop that will settle on what's likely some sort of sugar or carbohydrate. If you eat some of that fast enough before it degrades and oxidizes, you might get a good trip, but you won't be able to store it and keep it for use for very long without it turning inactive..

Edited by whatchamacallit, 08 June 2010 - 06:13 AM.

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#10 Cyaneus



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Posted 08 June 2010 - 05:42 PM

what's the most concentrated solution of psilly alcohol a person can make? Could you get it down to say, one or two cc's per dose? Than for the sake of convenience and safety you could just lace some cookies or sugar cubes with this alcohol (just like 'cid) and the complicated process of trying to reach crystals would be obsolete.

Also tagged with one or more of these keywords: crystal, extraction, methanol, wet, yeilds

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