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Help clarify the tao of rue extraction. I'm on the final base step Options
 
Jees
#21 Posted : 9/22/2015 5:41:28 AM

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pitubo wrote:
...Perhaps repeated washes of freebase precipitations cause much of the harmine to be washed away, leaving mostly harmaline behind? The freebases are slightly soluble in pH 7 water, harmine more so than harmaline...
I think it is the other way around, that with the FB water washes the harmaline will be first to start dissolving in the water.

Say you start to make washes and you end with pH of 9 then at that pH value:
harmine will be 95% FB (solid) and 5% will be in the wash water;
harmaline will be 14 % FB and already 86% will be dissolved in the wash water.

Freebase percentage AND pH calculator
 

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pitubo
#22 Posted : 9/22/2015 9:35:17 AM

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Oh yes, you're right. I made a mistake there, thanks for pointing out the correct facts.

This also means my theory about washes changing the color of freebase makes no sense.
 
sleepermustawaken
#23 Posted : 9/25/2015 12:57:52 AM

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Nereus wrote:
but i recall snozz confirming an analysis about leftover harmalas that precipitate upon basing the salt solution are relatively pure harmaloids.


I basified my discarded manske water and got over 7 grams of brownish freebase but they don't look like crystals, more like dried mud. In the sun I only see very few crystal shimmerings. Not sure if it's harmala, but what else could it be? The manske water was clear and no sediment was in there.

Heres the thing though, when I based the water what precipitated was cloudy and wouldn't sink it just floated. It looked like the jar in the middle:

 
Nereus
#24 Posted : 9/25/2015 8:06:58 AM

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Quote:
I basified my discarded manske water and got over 7 grams of brownish freebase but they don't look like crystals, more like dried mud. In the sun I only see very few crystal shimmerings. Not sure if it's harmala, but what else could it be? The manske water was clear and no sediment was in there.


Further repeating the steps will get your alkaloids even more cleaner. The first precipitation always yields a darker product but after time nr.3 the freebases are off white while the salts are a nice golden yellow.
 
Nereus
#25 Posted : 9/25/2015 8:14:41 AM

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Quote:
Heres the thing though, when I based the water what precipitated was cloudy and wouldn't sink it just floated.


Leaving it in the fridge for some time helps lots with settling them on the bottom of the jar.You can then decant and do a cople of repeated clean water washes to balance the ph of the water and get rid of any base contamination.
 
pitubo
#26 Posted : 9/25/2015 11:12:30 AM

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Be careful to assume that these are harmala alkaloids only. The Manske saltings are there to separate the harmalas from the vasicines. What precipitates after strongly basing the Manske filtrate could contain these alkaloids in increased relative amounts.

 
Nereus
#27 Posted : 9/26/2015 12:31:56 AM

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I've done tha salt water basing step after the 3rd stage of cleanup... i figured that by then maybe in 3 subsequent manske procedures the vasicine compounds might have stripped away.
 
sleepermustawaken
#28 Posted : 9/26/2015 2:42:00 AM

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Nereus wrote:
all that remains is maybe do a side by side bioassay of the two and try to tell the difference.


If only harmalas were soluble in a solvent and other alks wern't Sad

Trouble is, I filtered my mansked crystals through coffee filter... Based what came out the other end, it is possible that smaller manske crystals escaped and when I based they turned in to larger crystals and were cought by coffee filter... I have nearly 8 grams of it from 500g extraction (totally clean before manske)

As pitubo says it prob is other alks but we could know by knowing the actual alkaloid content by seed weight and making guesses as to what amount is harmala and what amount is vascine etc.
 
pitubo
#29 Posted : 9/26/2015 12:03:51 PM

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sleepermustawaken wrote:
Trouble is, I filtered my mansked crystals through coffee filter...

Next time, let the crystals settle in the refrigerator and decant the supernatant liquid after a day.

sleepermustawaken wrote:
As pitubo says it prob is other alks but we could know by knowing the actual alkaloid content by seed weight and making guesses as to what amount is harmala and what amount is vascine etc.

The problem with that approach is that alkaloid content can vary with different batches of seeds.
 
sleepermustawaken
#30 Posted : 10/3/2015 12:12:35 PM

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Nereus wrote:
...all that remains is maybe do a side by side bioassay of the two and try to tell the difference.


Have you tried this yet? I have almost 10 grams of salted harmalas and ten grams of the stuff that would not salt but precipitated from basifying discarded manske water... Not sure if safe to eat. What IS this fricken stuff?!?!?

pitubo wrote:

sleepermustawaken wrote:
As pitubo says it prob is other alks but we could know by knowing the actual alkaloid content by seed weight and making guesses as to what amount is harmala and what amount is vascine etc.

The problem with that approach is that alkaloid content can vary with different batches of seeds.


Yes, i see that now
 
pitubo
#31 Posted : 10/3/2015 12:38:43 PM

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To complicate matters, in a number of those studies they used only methanol for the initial extraction of the seeds, which I expect to be very suboptimal. The studies that found larger amounts of harmalas used 1:1 methanol:water to do the initial extraction. The numbers in the methanol-only studies may well be off.
 
sleepermustawaken
#32 Posted : 10/5/2015 2:20:40 PM

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pitubo wrote:
To complicate matters, in a number of those studies they used only methanol for the initial extraction of the seeds, which I expect to be very suboptimal. The studies that found larger amounts of harmalas used 1:1 methanol:water to do the initial extraction. The numbers in the methanol-only studies may well be off.


Thanks, do you have any idea what that gunk stuff could be?
 
TGO
#33 Posted : 10/5/2015 6:07:11 PM

Music is alive and in your soul. It can move you. It can carry you. It can make you cry! Make you laugh. Most importantly, it makes you feel! What is more important than that?

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This might be what it is...MIGHT is the important word...Very happy

69ron wrote:
Let me say this again. Salt is SODIUM CHLORIDE. Sodium carbonate is a SODIUM. Both are SODIUMS. Water can only hold so much SODIUM. This is the problem.

If the initial alkaloids are contaminated with too much SODIUM chloride then adding more SODIUM carbonate will cause SODIUM to precipitate out with the harmalas.

Because SODIUM carbonate is less water soluble than SODIUM chloride, then SODIUM carbonate precipitates out, so you'll get harmala alkaloids that taste like SODIUM BICARBONATE because there's sodium carbonate in it.

It's simple chemistry. Water can only hold so much sodium. If there’s too much sodium chloride, added sodium carbonate will not dissolve.


Came from this thread: Suspiciously High Yield

I am by no means a chemistry expert but you said you based your discarded manske water (salt water). What did you base with? Sodium hydroxide or sodium carbonate? Either way, to me, it stands to reason that the above quote may prove true because they are both Sodium and as Ron pointed out, water can only hold so much sodium. He was talking about sodium carbonate though and I do not know if the same applies to lye.

And if I am far off, I would love for someone with more chemistry knowledge to please tell me why! Very happy

Hope this helps... Razz
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One Fish Two Fish Red Fish Blue Fish

 
Jees
#34 Posted : 10/5/2015 7:24:27 PM

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That time I based my resting manske water, that was with lye. It gave a nice white layer at the bottom but was a slime. Lye could not have precipated then.

Q: What could be it?
A: rue - [mansked rue]
Period.
No?
Big grin

TGO, that link, this guy putted a based rue (sodium-carbonate) in the freezer, that's really asking for sodium carb to fall out. The solubility of sodium carbonate rockets down with colder temps, even without NaCl salt. With NaCl even worse.
The only time you need a fridge on rue tea is manske, it has no use when going for the FB fall-out. Was he mixing up the idea?
 
TGO
#35 Posted : 10/5/2015 7:54:00 PM

Music is alive and in your soul. It can move you. It can carry you. It can make you cry! Make you laugh. Most importantly, it makes you feel! What is more important than that?

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Ah, okay well that is good to know! Smile

The very first time I ever extracted rue, I put in WAY too much salt during the first manske, leaving me with enough salt contamination that when I re-dissolved goodies/acidified and then basified, my sodium carb wouldn't dissolve fully which then left me with a bunch of sodium carb contamination (which was cleaned up later, of course).

So my thought process was that maybe if his water was salty enough, it may have been the base precipitating. I don't really know anything definitive, I was/am just spit balling ideas!

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Nereus
#36 Posted : 10/5/2015 8:43:17 PM

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Quote:
Have you tried this yet? I have almost 10 grams of salted harmalas and ten grams of the stuff that would not salt but precipitated from basifying discarded manske water... Not sure if safe to eat. What IS this fricken stuff?!?!?


Nope i did not have the time needed to wrap my head around it.Also figured I will not save it any longer since my time was limited, fridge space and somewhat unpatience towards the clean up process of it and titanic filtering job.I did actually save the best part out of my extracts and was very thankful with the results.Cool
 
Jees
#37 Posted : 10/5/2015 9:12:41 PM

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The Grateful One wrote:
... I was/am just spit balling ideas!
And I am glad you did! I had no idea before that NaCl salt had such an impact on the Sod-carb solubility, I've learned too. Thumbs up

Nereus, cool vids Thumbs up
 
Nereus
#38 Posted : 10/5/2015 9:30:51 PM

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Thanks Jees, foolish of me to have taken 'em down as I've lost a lot of data lately including those nice lapses.Will make sure to upload some back if I'll get my hands on some more.
 
sleepermustawaken
#39 Posted : 10/6/2015 3:15:01 AM

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Jees wrote:

The only time you need a fridge on rue tea is manske, it has no use when going for the FB fall-out. Was he mixing up the idea?


Not true for me, if I leave it room temp the alks stay on top and in the middle... in the fridge they sink to the bottom straight up, like a boss.
 
sleepermustawaken
#40 Posted : 10/6/2015 4:58:45 AM

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Just wondering though, if the manske water is yellow and then is basified... The sodium comes out dark brown? What makes sodium dark brown?
 
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