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simple titration, and dual solvent crystalization

Migrated topic.
foaf is a member here. he wrote up the first stb tek on the web

1kg dried cacti skins- powdered

add to 5 gal bucket with 3-4 gallons of water
with paint mixer on a power drill mix the cacti/water as slowly you add 1-2 lbs lye.
glasses/goggles. gloves etc are a must- base burns hurt
now let the mix sit for 12-24hrs or until it has turns completely watery (lye digesting the pulp)
i like to keep things warn during this stage. set bucket in large tub- and periodically add boiling water to tub to keep the bucket hot.
add xylene or toluene gently mix. siphon off w/clear tubing


here are notes from the last run:
took partially dried out cacti
blended w/minimal water
boiled until it stopped foaming- it was about 4gal of material
added to 5gal bucket w/2 lbs lye added slowly while rapidly blending w/paint mixer
material became watery in 1hr
added xylene toluene mix- blended again
separated quickly and did 4 pulls in 4hrs
salted w ph down used very hot water bath and funnel/cotton ball to separate and filter all the saltings
reduced volume on gas range set to high
added acetone
yield 10+ grams
 
thanks for the swift reply foafs tek sounds nice and easy..

couple of questions how much of the xylene/toluene mix do you add per pull? im guessing around a litre?

and can the xylene be substituted for limonene?

and 1-2 lbs lye is big difference! ive heard more is better for breaking up the mucilage so im guessing closer to the 2lb mark is better..

also in regards to your addition could you theoretically keep pooling lots of saltings then reduce and crash a load of them all out with the acetone in one go or would it be better to do them in sperate batches?

:thumb_up:
 
highRvibratoryfreq said:
and can the xylene be substituted for limonene?

also in regards to your addition could you theoretically keep pooling lots of saltings then reduce and crash a load of them all out with the acetone in one go or would it be better to do them in sperate batches?

:thumb_up:
Click to expand...


xylene is a suitable nps

(EDIT - for all saltings minus sulphate)
you can pool all saltings and evap them all, however nothing will crash out. the acetone is used to wash them of residual nps AFTER the alkaloids are anhydrous. please correct me if im wrong
 
yes puma in this case you are wrong...
once the water/salting(s) are reduced to a minimal amount of water you add acetone and watch the crystals grow in the mix of water/acetone.

this only works w/sulphate salts.

i dont recomend using d-limo. but it will likely work (as long as the acid you are salting with is very dilute-)
 
thanks again for all the great info ill stick to the xylene it worked well in the past for getting the jungle spice out of my mhrb. i just cant stand the smell of it like most people!

and is 1 lite of xylene per pull a good amount to use?
 
us gal.

i never measure anything really accurately- its not like baking a cake.....
 
Cool thread dg. Thank you.

Pardon my ignorance, is this h20/acetone freeze precip a new discovery?

dg said:
once the water/salting(s) are reduced to a minimal amount of water you add acetone and watch the crystals grow in the mix of water/acetone.
Click to expand...

Can acetone be safely reduced in a food dehydrator?
 
not really. i've been telling people about it for a few years now. the end material is really nice and pretty easily achievable

my dehydrator has just an exposed element electric not sure i'd evap acetone in it.
 
Is there any advantage to using HCL over Sulphuric? Seems like the pH down aquarium drops are easy to use. About how many drops does it take to get the ph to 7 during salting ?
 
cyantific said:
Is there any advantage to using HCL over Sulphuric? Seems like the pH down aquarium drops are easy to use. About how many drops does it take to get the ph to 7 during salting ?
Click to expand...

if you follow most "teks" hcl has the advantage. all that extra acid the teks call for will evap away. sulphuric acid doesn't evap- so if you overshoot it wont dry out.

the more alks in your nps the more acid you will need to add to bring the water layer down to ph6/7. test-add drops of acid-shake-test-etc
 
dg said:
sulphuric acid doesn't evap- so if you overshoot it wont dry out.
Click to expand...

Does the wash h2o/tone recrystalization wash away residual sulphuric acid ?

apologies if this was answered, does this method clean mesc acetate?
 
thats why you titrate- so there isn't any excess acid
this method makes mesc sulphate
 
cyantific said:
dg said:
sulphuric acid doesn't evap- so if you overshoot it wont dry out.
Click to expand...

Does the wash h2o/tone recrystalization wash away residual sulphuric acid ?

apologies if this was answered, does this method clean mesc acetate?
Click to expand...
No residual sulfuric acid wont evap and when you go to add water/acetone to recrystallize it will contaminate your solution and lead to problems of crystals not crashing out. Like dg says.. titration is definitly the way to go so there isnt excess acid.

Great recipe btw dg may give it a try :) You should really consider making a wiki page of this tech.
 
dg said:
i dont recomend using d-limo. but it will likely work (as long as the acid you are salting with is very dilute-)
Click to expand...

Having only performed 69ron's d-limo extraction thus far, d-limo is the only NP I have available. I am guessing this incompatibility is due to the reactivity of the alkenes in limonene with strong acid?
 
Precog said:
dg said:
i dont recomend using d-limo. but it will likely work (as long as the acid you are salting with is very dilute-)
Click to expand...

Having only performed 69ron's d-limo extraction thus far, d-limo is the only NP I have available. I am guessing this incompatibility is due to the reactivity of the alkenes in limonene with strong acid?
Click to expand...
Correct. If you over-titrate your saltings then the excess acid will pull garbage from the d-limonene.
 
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