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honey oil/purification

  • Auteur de la discussion Auteur de la discussion remo
  • Date de début Date de début
R

remo

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used the old school solvent extraction.. reflux soxhlet, and seperate w/ non polar. pet. ether. beautiful dark gold oil. but ready to isomerize . Can you advise on best Method??? base or acid . will using activated charcoal do any more then make dark gold into red????
 
"This stage rotates all the existing lesser cannabinoids and cannabinols into
THC, and all the existing THC into the most active isomer, delta-9-THC. This
step involves the use of sulfuric acid, so I shouldn't have to remind you to
wear long rubber gloves, don't inhale its fumes, DON'T TREAT IT CASUALLY
BECAUSE IT CAN EAT HOLES IN LOTS OF THINGS, INCLUDING YOU.

Dissolve the extract in 10 times its own weight in ether. SLOWLY, add one drop
of sulfuric acid for each gram of extract, stirring with a glass rod. Heat as
in the initial extraction, with the jar covered by a watchglass. Cook two
hours, stirring occasionally, and allow to cool.

Mix the solution with an equal volume of cold water and one-half its volume of
cold ether, and repeat the shaking and separation steps. Take extract and
slowly add the calcined ash from the first extraction. Stir it all in, and run
the solution through filter paper to strain the ash sediment out. Check for
any remaining acid by adding a small pinch of sodium bicarbonate (baking
soda). If the solution fizzes, keep adding bicarb very slowly until fizzing
stops.

Add fresh water and ether, shake and separate. Cook at 104F until the ether is
evaporated. Voila! You now have essence of cannabis, which can contain
anywhere from 85 to 99 percent THC"


found that at erowid......

__________________________________

and this at cannabis culture-


The potency of marijuana can be increased by about 50% simply by simmering a water slurry of the material for 2 hours. Add water as necessary to maintain the level. Cool and filter the mixture, and refrigerate the aqueous solution. Dry the leaf material at low heat. Drink the tea before smoking the marijuana. The effects are much more intense and last longer than those from the untreated leaves. The boiling water treatment isomerizes the inactive CBD, and decarboxylates THCA to THC.

Although Cannabidiol (CBD) has no psychoactivity, it does antagonize THC and produces other valuable sedative, antibiotic, and anti-epileptic effects. CBD can be isomerized to THC. If the plant is Phenotype III (containing mainly CBD in its resin), isomerization can double the yield of THC.

The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it. Isomerization can be accomplished with any of several solvents and acids. Alcohol and sulfuric acid isomerizes only 50-60% of CBD to THC; p-TolueneSulfonic Acid (p-TSA) in petroleum ether or other light, non-polar solvent will convert 90% of CBD to THC upon refluxing 1 hour at 130° F. (16, 17)

Reflux 3 gr CBD in 100 ml dry benzene for 2 hours with 200 mg p-TSA monohydrate until the alkaline Beam test (5% KOH in ethanol) is negative (no color). The Beam test gives a deep violet color with CBD. Separate the upper layer, wash it with 5% sodium bicarbonate, wash again with water, and strip the solvent. The remaining viscous oil should give a negative reaction to the Beam test. The crude THC can be purified by distillation (bp 169-172° C/0.03 mm), or by chromatography in 25 ml pentane on 300 gr alumina. Elute with pentane 95:5 ether to yield fraction of CBD and THC. Combine the THC fractions and distill (bp 175-178° C/1 mm).

Reflux 2 gr CBD in 35 ml cyclohexane, and slowly add a few drops of sulfuric acid. Continue to reflux until the Beam test is negative. Separate the sulfuric acid from the reaction mixture. Wash the solution twice with aqueous sodium bicarbonate, the twice again with water. Purify by chromatography, or distill (bp 165° C/0.01 mm). Any unreacted CBD can be recycled.

Another method is to reflux a mixture of 6 gr dry pyridine hydrochloride and 3 gr CBD at 125° C until the Beam test is negative. Wash the reaction mixture with water to remove the pyridine, then extract the mixture with ether. Wash the ether with water, evaporate the ether, and distill the residue i.v. to yield pure THC.

Similarly, reflux 3 gr CBD in 150 ml ethanol with 50 ml 85% phosphoric acid until the Beam test is negative. Work up the reaction mixture, and purify the THC.

Alternatively, reflux 3 gr CBD in 100 ml absolute ethanol containing 0.05% HCl for 19 hours. Extract the ether, wash the ether with water, dry, evaporate, and chromatograph on 400 gr alumina to yield


I remember seeing hexane as a superior solvent. Hexane's got to be everywhere......hobby store
 
Drink the tea before smoking the marijuana.

That's not such great advice... just a lot of chlorophyll and plant waxes etc in there. Sounds like a bad stomachache waiting to happen...

But I enjoyed the isomerization parts. No chem geek who likes cannabis can resist the idea of an isomerization in lab glass.

Sorry about the semi-vacuous post, but I'm new here and I need to get to 20 posts so I can get my PMs! :)

MM
 
remo: sorry guy, I didn't address your question and should have. What I have read regarding your question is that multiple passes through charcoal will get it progressively lighter in color, all the way through to very light gold like honey if you wish; however, you will have losses on each pass. So your light gold oil may end up being 50% the volume of dark oil you started with.

cheers
MM
 
sounds like lots of agro to me.. For maximum stone I just used to make bubble hash from my trim. That used to smash me to pieces! I can't see why someone would want to be any more stoned than how you are on bubble hash, although I've always been a bit of a lightweight!!

igt
 
That is alot of work for some oil but the isomerization bit looks interesting :)

For quick and easy oil :)

I suggest you find a smallish decent cylindrical vessel with one end having a screw on lid, Then piercing 4 -8 small holes in the end that is solid. Then pierce a very small hole in the top of the lid, Then buy as much butane lighter gas as you need, Say a tin a run / fill of vessel. Get a pyrex dish and take yourself to an easy to ventilate area that has no ignition sources including electricals. Get 2-3 tea bags depending on the quality of the filter paper used and empty the contents completely, Cut a circle out of them all and place as many in as you think you need in the vessel. Fill with plant matter, Point small holes at pyrex dish and pump butane thru the lid, I find it best to put an adapter on to create a good seal. Collect the butane as it comes out the filterd end in the pyrex dish and allow to evaporate which doesnt take long at room temperature, Allow for any moisture that may have been in the butane to evaporate too. Collect up the honey oil and enjoy :D

P.S. Your vessel should be big enough to hold maybe an oz at a time, A big vessel means you cant get the pressure to build up that you require for extraction. Also your plant matter works best dry :)
 
i cant verify this is any good as an alternative buuuut here the post..

""1) Dissolve the BHO in 10 times it's own weight of naphtha (petroleum distillates, i.e.: lighter fluid - Swann was the cleanest I found when doing the DMT).

2) Acidify to PH2.0 (oxalic acid) then heat gently for 2 hours in a pyrex beaker with a glass lid (to allow some of the pressure but little of the naphtha to escape) on a hot-plate OUTSIDE, preferably in a double boiler. Let it cool completely.

3) mix with an equal volume of water and half volume of naphtha and mix.

4) Allow to settle then seperate the naphtha layer (this has the goodies in, never chuck the naphtha, always the other part).

5) Add ash from heating the plant material you extracted the BHO from (once it has totally dried off any trace of butane) until only white ash remains. Filter out ash with a coffee filter and add bicarb until it no longer fizzes.

6) add water and half volume of naphtha once more, allow to seperate and drain off naphtha layer.

7) Evaporate naphtha. This doesn't have to be done by boiling, just warming gently, maybe with the hot-bath method you use on the BHO to drive off the butane. It will obviously take a fair bit longer, but is less risky.

You should be left with isomerized Honey oil.



dont try it till someone knows for sure i copy n pasted for discussion

how viable is making delta-3-thc from pulegone and olivetol?
 
Is there any reason one couldn't extract w/ ISO and lower the pH w/ HCl and then neutralize w/ baking soda and then filter and evap?
 
..yeah i usually just rinse thoroughly with isopropyl alcohol, and sit to evaporate or u can brew it off carefuly (never with open flame).
i wanna try extract with butane. then add a little iso. to clean it and evaporate.
 
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