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Sodium carbonate for harmala xtraction - too low ph? loss of yield? Options
 
endlessness
#1 Posted : 3/2/2012 4:10:48 PM

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So recently i've been checking the pH during harmala extractions, and noticed that sodium carbonate harmala solutions are only going up to 8.8 or so and sodium bicarb up to 7.8 or so... This would mean a significant part of harmaline is being left behind, as you can check in the freebase percentage pH calculator thread even after adding sodium carbonate up to saturation point.

This is weird because in theory sodium carbonate would take pH up to 11.6, and my pH meter is calibrated... So can anyone els with a pH meter double check what pH you can get with a sodium carbonate solution (or if youre extracting harmalas, checking the pH of the harmala solution after adding sodium carbonate) ?

So while we dont get this issue settled, here's what I would recommend for all those extracting harmalas: After precipitating with sodium carbonate and decanting/filtering to retrieve the harmalas, dont throw the solution away, and add to the solution some lye or a strong base like KOH, to precipitate the rest of harmaline.


EDIT: IGNORE THIS POST.... I had just not converted the sodium bicarb to carb properly, now I did it again and it goes up to ph 11+
 

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amazingino
#2 Posted : 3/25/2012 5:21:01 PM

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I would like to know the answer to this too as I only have sodium carbonate at hand Smile
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soulfood
#3 Posted : 3/25/2012 6:14:41 PM

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I've been doing 3 precips on my harmaloid extractions. NaHCO3, then Na2CO3 and then finally with NaOH.

When the solution has been thoroughly precipitated from it's pretty much colourless, but for a couple of years I had been discarding yellow liquids after the Na2CO3 step. Sad
 
NamRa
#4 Posted : 4/9/2012 2:58:49 PM

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I got my sc carbonate water upp to 11.5 with maybe a gram of sc
 
Infundibulum
#5 Posted : 4/9/2012 3:49:10 PM

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It's a different thing changing the pH of plain water (just as NamRa) did and changing the pH of a complex solution, like one that has harmine, harmaline and whatnot. I remember once I tried to basify a cactus acidic solution and after copious amounts of NaOH I couldn't get it higher that 11 or so, that stroke me as very peculiar. My pH meter was calibrated alright.

The thing is that a solution of a weak base (like harmine) and its salt (like harmine -HCl) already conforms with the definition of buffer. Add to the mix another weak base like sodium carbonate and the solution can have truly difficult to predict properties - what is more, sodium carbonate/sodium bicarbonate mixtures are also commonly used for buffering (see attached paper so go figure....in these cases only a stronger base/acid can be employed to change the pH.

Endlessness, do you have first-hand observation of more harmaline precipitating out after upping the pH with a strong base like KOH or NaOH (that is, after having upped the pH with bicarbonate to get the harmine, then upped again with carbonate to get the harmaline)?? I would imagine that in this scenario any furtehr precipitation would be negligible, as in these pH-dependent precipitations the law of conservation of mass of Lavoisier may be more applicable.




Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
cyantific
#6 Posted : 7/12/2012 9:57:06 PM

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I tried using sodium carbonate after vinegar in a rue extract. I was only able to get my ph to go up to 10.5. I had to add some NaOH to get to 12.5. (with a freshly calibrated meter) I'm not sure if the ph needs to get above 12 to release all the alkaloids?

What's a good way to make sure there's no lye left in your final product?
 
endlessness
#7 Posted : 7/12/2012 11:09:24 PM

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A sodium carb wash should get rid of lye and should not lose much product

The other day I tried this again and was able to get the pH up to 11 with sodium carb, I think my sodium carbonate was just not properly converted when I first did this, probably didnt heat for long enough. Did you make your sodium carbonate yourself by heating baking soda?
 
cyantific
#8 Posted : 7/13/2012 3:42:50 AM

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endlessness wrote:
Did you make your sodium carbonate yourself by heating baking soda?


I purchased the Sodium Carbonate pictured below.

Can you outline the process of a Sodium Carb wash?

Thanks!
cyantific attached the following image(s):
soda_ash.jpg (51kb) downloaded 455 time(s).
 
endlessness
#9 Posted : 7/13/2012 8:58:49 AM

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Instructions for washing are in the FAQ.

Yeah this sodium carb should be good.... Maybe its just that your solution was quite concentrated and hence there were a lot of "buffers" which made it difficult to raise the pH past a certain point.

Did you add the sodium carb straight, or did you do a saturated sodium carb solution and add that to the rue solution? I find this second option works better
 
cyantific
#10 Posted : 7/13/2012 6:08:35 PM

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I dissolved the Sodium Carb in hot water first, then added it to the rue solution.

I've just been washing the alks with plain water, as outlined in the Gilbran2 cappi tek untill the ph drops to 8.0 Is there any advantage to washing with Sodium Carb over plain water?
 
mew
#11 Posted : 7/14/2012 8:06:30 AM

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no, as long as the solution dosent start to dissolve the alkaloids. if it does add basssssss
 
cyantific
#12 Posted : 7/14/2012 6:34:20 PM

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endlessness wrote:
I dont think sodium carb wash removes a lot of oils, it would remove polar compounds (like lye) As long as the water is slightly basic it will wash it out.


Just found this bit of info.

It seems washing with Sodium Carb does have an advantage over plain water wash.

 
 
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