Simple manske on rue tea(results)

[TGO]

That is a brilliant edition to the squeeze method, Jees! I don't know why it never dawned on me before now to contain the seeds in something while they boiled.

:thumb_up:

 

[Sakkadelic]

I think i was wrong about about the impurities part cz i forgot that the 6% yield was just for freebase and 7.1% was for HCl.. i deleted that part

I tried to purify it more and got beautiful results
I freebased 1g of HCl harmala and got 800mg fb, the equivalent of 930mg HCl, i'm sure i lost few mgs spilling some drops of the concentrated hcl solution and impatience with precipitation but that's fine
I salted the freebase and did a manske
Got 540mg of the most beautiful golden needles i've ever got but the rest 390mg refused to crash out for some reason
So i based the filtered solution and washed 3 times with water and got 320 mg of the most clean freebase i've ever got, the equivalent of 372mg of HCl
So in total i got the equivalent of 912mg of HCl 6.4%

Next time I'll do a 6th boil or do 1 freeze/thaw before the first boil plus applying the jeezbagtek, maybe i get closer to that 7.1% of high purity.

 

[Aum_Shanti]

That looks really nice! So pure... :thumb_up:

But I'm still a bit puzzled about the numbers.
E.g. as I read from Fritzsche, the yellow HCl is actually the HCl hydrate. So the pure HCl would actually weigh something like x0.87 of the yellow stuff.
BTW: The pure HCl isn't yellow anymore but also white.

So from this I would expect, if you have yellow HCl, that in theory one would first have to calculate the non hydrate weight (about x0.87) and then calculate the FB (about x0.85).
So in total a correction factor of about x0.87x0.85=0.74

So from this POV 1g pure yellow HCl should yield 740mg FB in a 100% conversion.

I'm definitely still at my own tests and didn't verify the numbers from Fritzsche. But I would expect them to be more or less accurate.

How did you dry your HCl and FB before weighing?

 

[Sakkadelic]

The HCl i always dry with hair dryer on hot, and this time i finished the drying of the original 2.44g yield next to a heat source until the chips became hard and the weight stopped decreasing so my HCl should be dehydrated, Right?
The freebase i dry using a fan sometimes under the sun or i finish it in the oven but always got the same results but in this last experiment it was dried using just a fan.
About the color i think you misunderstood the book, this is from the book you posted part "On Harmaline. By J. FRITZSCHE."

Harmaline.—In the pure state it is quite colourless, but it is usually obtained of a somewhat brownish colour. To obtain it per fectly pure, it is diffused in water, acetic acid added until the greater portion is dissolved ; the filtered solution diluted, and precipitated with nitrate of soda, chloride of sodium or muriatic acid, up«n which it is again filtered, and the salt, after being washed with a solution of the precipitant employed, dissolved off the filter with lukewarm water. The solution is digested with animal charcoal till it possesses a light yellow colour; it is then precipitated, whilst still hot, by an excess of caustic potash. If the precipitate is not perfectly white, the same operation must be partially or wholly repeated ; and even then the preparation usually acquires a brownish tint on filtration and washing, especially when ammonia has been employed instead of potash to precipitate it. This colouring is undoubtedly owing to the influence of the oxygen of the atmosphere. The harmaline thus obtained forms broad laminar and scaly crystals of pearly lustre, which are of larger size the more slowly the precipitating agent was added.....

Hydrochlorate of Harmaline.—This salt is most readily obtained by precipitating the acetate or sulphate of harmaline with chloride of sodium, in a solution of which it is sparingly soluble ; but it is still more advantageous to use hydrochloric acid to precipitate the acetate of harmaline, in which the hydrochlorate of harmaline is nearly insoluble. If the salt, after washing it with hydrochloric acid, does not possess a light yellow colour, it may be purified by dis solving it in cold water, and again precipitating it with dilute hydro chloric acid. The hydrochlorate of harmaline forms long, slender, prismatic crystals of a yellow colour, which contain 4 equivs. water, part of which however it readily loses. It dissolves pretty easily in alcohol and water. On analysis, it yielded......

So it's obvious in the first line he is talking about the freebase and the alkaloids are finally precipitated with caustic potash or ammonia so it's the freebase not the HCL

And the second part "the hydrochlorate of harmaline forms long, slender, prismatic crystals of a yellow colour" and he also says that if the solution is not yellow it should be purified more
So the color of pure HCL harmalas is yellow

Another thing he mentioned is "which contain 4 equivs. water, part of which however it readily loses." So the HCl hydrate is easily dehydrated probably even without heat.

 

[Aum_Shanti]

Actually I meant another excerpt (p479) on Harmine HCl:

When dried in the air,[...] it contains 4 atoms or 12.38% of water of crystallization, and is of yellowish color; at 212° (probably F?) the water escapes, and the salt becomes white.

(212°F would be 100°C, so I would think he probably meant Fahrenheit.)

And the second part "the hydrochlorate of harmaline forms long, slender, prismatic crystals of a yellow colour" and he also says that if the solution is not yellow it should be purified more
So the color of pure HCL harmalas is yellow

I think he just relates to the HCL state in this tek of being yellow. As you would obviously have to dry them in the oven to make it anhydrous.

Another tek, making it anhydrous would be e.g. acetone or as Fritzsche says also a strong alcohol.

I usually dry my hair dryer dried FB in the oven (at 200°C). But I always see quite a weight difference, if I do that. But that's surely dependent a lot on your drying teks.
For me personally hair or fan drying until complete dryness is no option, as the dry FB is so fluffy that a lot of it would just fly away...

 

[Sakkadelic]

Hair dryer is not good for drying freebase but using a fan and slowly drying overnight, the freebase will not fly away, it will just dry and harden and then you can scrape it and powder it.. i only use hair dryer on HCl crystals enclosed in the coffee filter
Can u link the book you are referring to here, i didn't find anything about the color on page 479 in the books posted in the Original Manske/Hasenfratz (Fritzsche) thread you made..

 

[Aum_Shanti]

You can download it from my original thread here:

Original Manske/Hasenfratz (Fritzsche) Extraction procedure - Collaborative Research Project - Welcome to the DMT-Nexus

I would think that Fritzsche probably is right here, as in Phlux's thread (Possible new tek for almost anything - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus) he got white stuff as the citrate salt, which I at first mistakenly took as being FB, because it was white.

Only then I realized that it seems only the hydrates are yellow.
From Fritzsches indicated weight, it seems these are dihydrates.

 

[ijahdan]

Just made a new batch of rue tea and on reading this thread, Im considering omitting the first basing stage and going straight to the manske, then repeating a few times to clean the alks, then base, separate etc. Seems quicker and easier. Or am I missing something?

 

[Sakkadelic]

Just made a new batch of rue tea and on reading this thread, Im considering omitting the first basing stage and going straight to the manske, then repeating a few times to clean the alks, then base, separate etc. Seems quicker and easier. Or am I missing something?

Sorry i didn't see this on time, yes it's quicker and easier just make sure the tea is saturated enough to get all the alks out
What did you end up doing and how did it go?