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Swims Peganum Harmala Extraction

Migrated topic.
swim took a batch of dirtyish freebase from the cleanup op - washed it with basic water then crystallized it in acetone - no reddening but it was noticed that there was either 2 kinds of xtals (dark spikey ones & flat clear ones) or dirt on some xtals or a different formation type to the rest - no harmala red was noticed - swim wants to know now how to separate the harmaline from the harmine without using alcahol as swim has none of that - dlimonene ? any ideas ?
 
^^You could take advantage of the difference in pka. Harmine is about 7.07 or 7.45 (seen both reported) and harmaline is 9.55. pka is the pH at which a substance exists half in its ionized form and half in its freebase form. So if you keep the pH below 8.5 or 8 and you extract with a non polar solvent the harmine will dissolve but the harmaline won't and at pH above 9.55 harmaline will dissolve (so will harmine unless its removed first).

There is also chromatography but thats rather advanced but if you want to let know more ask.
 
if harmaline or hamine is mixed with a base - wont it precip out as soon as the ph goes up as in basing in the manske - say swim disolves his harmaloids in water then pushes the ph up to 8.2 - wont the harmine just drop out - ? - would swim have to use a solvent - ? if so what solvent ?
 
thanks man - swim will make the solution and has the perfect way to filter it to catch the solids
its crude but it works well - the plunger and needle are removed from a syringe, a perfectly fitting disk is cut out of a coffee filter and fitted - most of the clear liquid is decanted and filtered first - quick - then the muck.
When most of the liquid is out the plunger is put back in and the remaining liquid is pressed out by the air pressure when the plunger is pushed, - the collected solids are carefully removed by tapping etc to produce a tablet which should be chopped and dried further.
after this swim will try to rextalize again to see if this solved the issue.
 
Fuego said:
a better way of cleaning your freebase is to just add it to water let it settle to the bottom, decant, add more water, so on until the water is clear. your freebase will be rediculously clean :D
Can someone confirm this please ron or burnt?
 
Big Inhale said:
Fuego said:
a better way of cleaning your freebase is to just add it to water let it settle to the bottom, decant, add more water, so on until the water is clear. your freebase will be rediculously clean :D
Can someone confirm this please ron or burnt?
The water should be basified otherwise you loose product!
 
kemist said:
Big Inhale said:
Fuego said:
a better way of cleaning your freebase is to just add it to water let it settle to the bottom, decant, add more water, so on until the water is clear. your freebase will be rediculously clean :D
Can someone confirm this please ron or burnt?
The water should be basified otherwise you loose product!
How much loss are we talkiing about?
 
swim washed with basified water and the only loss was a loss of impurities (the water was basified with sodium carbonate)
 
swim mixed about 2 teaspoons of sodium carbonate in about 100ml warm water to make the basic solution - no idea - sodium carbonate is really a much nicer base to work with.
 
Phlux- said:
swim mixed about 2 teaspoons of sodium carbonate in about 100ml warm water to make the basic solution - no idea - sodium carbonate is really a much nicer base to work with.
So you think one tablespoon of lye would be sufficient since its stronger.
 
1tbs lye to 100ml water would give you a very very strongly basic solution - perhaps too basic, could even possibly burn you - got anything against using bicarb or soda thats been baked in the oven - it really is a usefull thing to have around, its safe, etc...

when swim finishes his lye he will never buy lye again, sodium carbonate and calcium hydroxide seem to function perfecly and are far safer.

is there any extraction application where lye is required and the other 2 i mentioned wont cut it ?
 
One wouldn't dump the lye. This bloke used it with quiet a succes.
bluejay said:
grind seed,,,soak in HCL water,,,filter,,, raise ph to 12 via lye water,,,let stand,,, vacuum pump out water,,,,pour in ph 12 again 2 more times,,,settleing after each time,,, now pour in straight hcl,,crystals dissolve and realse junk that was captured within them,,hcl water will be dark again,,,,raise ph to 12 and just keep doin this,,,take about a week and a half to run one jar,,hence running many at a time...
not sure what pH has the initial soaking HCl water. It could be possible that extreme pH may break down those gums and oils which making filtration so difficult
 
Phlux- said:
1tbs lye to 100ml water would give you a very very strongly basic solution - perhaps too basic, could even possibly burn you - got anything against using bicarb or soda thats been baked in the oven - it really is a usefull thing to have around, its safe, etc...

when swim finishes his lye he will never buy lye again, sodium carbonate and calcium hydroxide seem to function perfecly and are far safer.

is there any extraction application where lye is required and the other 2 i mentioned wont cut it ?
I have nothing against it I just dont have it and I have a good amount I would like to use it up.So what would be a good measurement with Lye to water Using 5 grams of extract.
 
Big Inhale said:
Phlux- said:
1tbs lye to 100ml water would give you a very very strongly basic solution - perhaps too basic, could even possibly burn you - got anything against using bicarb or soda thats been baked in the oven - it really is a usefull thing to have around, its safe, etc...

when swim finishes his lye he will never buy lye again, sodium carbonate and calcium hydroxide seem to function perfecly and are far safer.

is there any extraction application where lye is required and the other 2 i mentioned wont cut it ?
I have nothing against it I just dont have it and I have a good amount I would like to use it up.So what would be a good measurement with Lye to water Using 5 grams of extract.


ehrmmm So you fancy pH of 12 with strong base NaOH. Very simple calculation
pH = 12, m NaOH = ?

pH =14 - pOH => pOH = 14 - pOH => pOH = 2

pH = -log c(OH) As I said NaOH is strong base so one can say c(OH)= c NaOH

Then c = 10 exp(-2) = O,o1 Sooooo.... desirable molar concentration is 0.01 mol/dm3 = 0,01mol/l

Where `c` is molar concentration defined as c = n/V where n is amount of moles in solution and V is volume of solution......

Then `n` is defined as n = m/M where` m `is weight of chemical compound (NaOH) and `M` is it`s molar mass [Molar mass of NaOH is M = 40 g/mol ]

Then c= n/v = (m/M)/V => c= m/MV

Then m = cVM then for NaoH m= 0,01.1.40= 0,4 g NaOH

SOoo result To create solution of NaoH at pH 12 one need add 0,4 grams of 100% NaOH in 1 liter of distilled water!
so easy with that lye, pal! :twisted:
 
soulfood said:
I need to learn how to make sense of that :?

It`s very simple son

funny thing would be if one try reach pH of 8 with NaoH

then molar concentration would be 10exp(-6) and calculated amount of NaOH in one liter of distilled water would be 0,00004g = 40 micrograms. :lol: ridiculous, that`s very little ammount that`s near to treshold dose of LSD
 
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