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1/2 the amount of Salt precipitates 1/2 the amount of Harmalas...

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plumsmooth

plumsmooth

Rising Star
After reading a couple of references or more to using less salt to get purer crystals:

I re-dissolved 1.1 gram Rue Harmalas into 100ml water.
I then dissolved 10 grams salt into 100ml hot water and added that to the 100ml rue harmala water.

In short, I cut the salt component of the Manske recipe in half.
10 Grams of Salt was added to 200ml water.

The result: Clearly very little harmalas precipitated.

Next I went back to the original formula and added another 10 grams of salt and reheated.
Now, 20 grams salt per 200ml solution.

The Result, at least Twice as many Harmalas precipitated, a much better anticipated viewing experience.

Conclusion: There is some confusion, or rather ambiguity regarding this formula.
The confusion arises through the use of Hot Water to dissolve and "saturate" the solution with salt.
Hot water holds a bit more.
For that matter, the original formula is probably achieved by only saturating 1/2 the "Hot" solution with salt.

In other words Hot, near boiling water, must hold close to twice as much salt if not more.
And considering room temperature water holds 37 grams per 100ml.

This idea of saturating hot water and adding it back in a ration of 1:1 Saturated Salt Water to Harmala Water is actually adding too much salt.
Since the recipe only calls for 10 grams salt per 100 ml solution.

I really don't see the point of guessing and eyeing it then.
Why not just follow the original recipe?
How much Salt contamination could there possibly be?

I guess that is the next experiment:
Although I am not a fan of Harmala Red:
Re-dissolve Manske Harmalas into Alcohol.
Decant any possible salt contamination (hopefully 99% ipa for example would hold very little).
Evaporate.
Proceed with the original Manske Formula.
Weight and compare yields to determine salt contamination once and for all.
 
Thanks for experimenting. I suspected that not saturating the entire solution but rather just part would yield purer crystals but some might not precipitate.

I would avoid that alcohol step. Why not just do normal manske with full saturation, and then redissolve the alkaloids in hot water and precipitate with base? Any salt contamination will not precipitate together with the base so you clean it up. Salt contamination is no problem at all if you clean up after by base-precipitaitng.
 
P.S. I believe the Harmalas I re-dissolved were Alcohol Cleaned.
They have that slightly darker tint.
I had forgotten about them in the pantry.

Therefore after re-weighing, if the yield is higher than 1.1.
This will suggest Salt Contamination?

I believe some loss is to be expected due to unprecipitated Harmalas or contaminants.
However this particular batch was cleaned at least 5 times total.
The color of the water even after collection is usually darker.
 
Why not just do normal manske with full saturation, and then redissolve the alkaloids in hot water and precipitate with base?
Click to expand...

Can one simply to a calculation based on Molecular weight difference to determine?

However, doesn't the Base have Sodium Carbonate residue?
 
The way I've been doing it is I use half the salt and it precips beautifully pure harmalas.

After I filter the harmalas out of the solution, I'll reduce the solution by half and precip again.

It takes a bit more work but the harmalas that precip are really nice and if you choose to not base them, I doubt there is any salt contamination at all.

I'll continue to do some tests when I can but so far I prefer using the half saturated solution instead of a fully saturated solution. To each their own I guess.
 
Melodic, may I ask, what do you mean by half the salt?
Do you mean half of a saturated solution?
Or half of the original Manske Recipe?
Because a saturated solution holds 36 grams per 100 ml h2o2.
So half of that would still be almost 100% more salt than the original recipe calls for.
half of 360 = 180 = 80% more... if my math is correct.

BTW, I also have to correct my original post.
Apparently water temperature has little effect on salt's solubility in water.

My main concern at this point is:
if deviating from the original Manske Formula what's the reason?

However, if someone is saying half the Manske original formula = still plenty of Salt:

Then I will try this again...

That would be 5 grams salt per 100ml solution...
That's a heck of a lot less than half of saturated which is 18 grams per 100ml...
 
You guys confuse me with all these numbers (or maybe im too stoned :p ) !!

Instead of weighing the amount of harmala manske-precipitated salts and supposing they are pure and comparing the yields as salts, why not doing the test with different salt amounts during manske, but then redissolve the harmala salts and precipitate with a base, and then compare yields (freebase wont have salt contamination and will be a much more accurate comparison)

Also in case less salt = smaller yield, you can always reheat the solution and add more salt to crash out the rest of alks + salt contam (and then redissolve and freebase to get rid of salt contam
 
When I say half the salt, I mean the technique I use in the Tao of Rue and the same technique used by Phlux- in the caapi manske xtals thread.

You dissolve your alks in a known amount of vinegar/water.
Completely saturate the same amount of fresh water with salt.
Add the solutions together and allow to cool.

I find that this gives the alks more water to grow in with just enough salt to push them out. If you use an excess of water/vinegar instead of starting with a saturated alkaloid solution in the beginning (eg. instead of using 20ml to dissolve a gram of alks, use 50ml) there is more room to grow.

If you allow the alks to finish growing completely, I've found that while there are still a few stray alks in the solution, it's not much at all. I'd bet that it's over 90%. You've got to allow the crystals to form completely though.

I kinda botched the last tests I posted about in the Tao of Rue thread but I will re-do them and document everything as I go to make sure it's as reliable and repeatable as possible.

I need to work with the original manske some more. I've only tried it once since you posted it and the precipitation from it seems to be a lot clumpier than using the technique I've been using from Phlux.

EDIT: Sorry for not answering the reason for deviating from the original manske.

1st reason why is because I was unaware of the original manske formula. I was only aware of completely saturating the entire solution which I never liked. And then recently I read the post from Phlux regarding doing the manske on the caapi. He had such good results that I tried it on rue and it worked just as well. So I've just kinda stuck with it since it works so well.
 
You dissolve your alks in a known amount of vinegar/water.
Completely saturate the same amount of fresh water with salt.
Add the solutions together and allow to cool.
Click to expand...

Anyway, I believe this is almost twice the amount of salt that is needed -- as explained in the previous post.

You guys confuse me with all these numbers (or maybe im too stoned ) !!
Click to expand...

I'm sorry to keep coming back to this.
But in essence, at this point, the discrepancy seems to lye in the differential between the original 10g per 100ml Manske recipe and complete saturation cut in half which equals 18g per 100ml.

But double actually; since my interpretation of the "TAO extraction" was misconstrued into confusing half of saturated with half of Manske.

In other words, 5g per 100ml is half the Manske and 18g per 100ml is half the Tao.
Now, may I ask, is the TAO half empty of Half full?
 
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