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put into a 500 ml flask along with a solution made up of 150 ml ethyl
alcohol, 150 ml water, and 100 grams KOH. Next, 15 ml of hydrazine
hydrate is added. This hydrazine should be the monohydrate, which is
64% hydrazine. If a weaker variety has been scrounged up, this can be
made to work by adding more, and using less water.
Now the flask should be fitted with a condenser, and flushed with
nitrogen. Then heat the flask in an oil bath to gentle boiling for 4
hours. A slow stream of nitrogen to the flask during the reflux averts
the danger from hydrazine.
The flask is next cooled, and the contents poured into a sep funnel of
at least 1000 ml capacity. The batch is then extracted with 600 ml
ether, followed by 600 ml of an 85-15% mix of ether and alcohol.
Finally, one more extraction with 600 ml of 85-15% ether-alcohol is
All of the desired product should now be extracted into the
solvent, and out of the water. This fact should be checked using a
black light to look for the characteristic blue fluorescence.
The combined solvent extracts should now be lowered to a pH of
about 2 using HC1. At this point, a precipitate should form, and it
should be filtered out. The precipitate should be washed free of
entrained product with 4-1 ether-alcohol, and the washing added to
the rest of the filtered solvent.
Now 2750 ml of water should be added to the solvent, and the
mixture placed in a gallon and a half glass jug or 5000 ml beaker. To
this should be added 3 portions of cation exchange resin in H* cycle.
Cation exchange resin is a common item of commerce used in
deionized water systems. Check the yellow pages under "water" and
see which of the local Culligan men offer deionized water systems.
The deionizers come in two-tank systems with one tank packed with
cation exchange resin to remove calcium, magnesium and sodium
from the water. The other tank has an anion exchange resin to remove
chlorides, sulfates, and so on. It is no great task to buy cation
exchange resin from these outlets. The resin consists of tiny plastic
beads coated with the exchanger. In the case of the cation exchangers,
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this is generally a sulfonate. "In H* cycle" means that the resin is
charged up and ready to go. This is generally done by soaking the
resin in 20% sulfuric acid in water for a while, then rinsing with
distilled water. Check the directions on the container of resin. Steer
clear of mixed resins that contain both anion and cation exchangers. If
the Culligan man is too stupid to know the difference, or doesn't
know what he has, keep looking until you find one who knows his
The treatment with three portions of cation exchange resin in H*
cycle should be done as follows: Each portion of resin should weigh
about 15 grams. The first portion is added, and then the mixture
should be stirred strongly or shaken for about 10 minutes. The product
will come out of the liquid, and stick
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