Harmala extraction, needles aren't forming, need a bit of advice?

[Volrux]

I found this letter in front of my door

"Hello there,
I am performing my first Harmala extraction, and I ran into an error. I think I know what went wrong, I will explain.

Before performing the Manske, it is required to add a hot vinegar/water solution to the harmalas. Later it is stated that an excess of vinegar/water in the solution would give needles more room to grow. (This is the tek I'm following: The Tao of Rue Extraction - DMT-Nexus Wiki)

I added the hot vinegar and water, filtered it a few times, and then saturated the same volume of hot water with approximately 50 to 75 grams of rock salt. Then I added the saturated water to the solution and let it cool down slowly.
It cooled down in about 7 hours, and now it's for over 8 hours in the fridge. But still no needles have formed?! :O What went wrong?

Because nowhere is stated how much hot vinegar you should add, I suspect I added a bit of a too much excess. I misjudged the insolubles for Harmalas and kept adding more vinegar. That was my mistake I think.

Now my question is: What to do? Should I double boil the solution and saturate with more salt? Or should I base with sodium carbonate/ sodium hydrogencarbonate/ sodium hydroxide to neutralize the excess of vinegar?

Please help me out "

 

[MelCat]

You should be able to reduce the solution by boiling it down. No need to double boil, harmalas aren't sensitive to heat when in solution. Once a good bit of the water/vinegar has evaporated, cool again.

From the tek in regards to the manske -

The first and the "official" way is:
Recommended
Take a note of how many ml's you have and add 10 grams salt per 100ml solution. Make sure your solution is hot before you add the salt, otherwise the harmalas might fall out too soon. Allow to cool slowly.

You said you added between 50-75g of salt. Reduce it down to around 500-600ml and you should be close to goal.

 

[Volrux]

Thank you very much! I will try and let you know if it worked. Thanks again for the quick answer!

 

[Jees]

I posted some tips here.

 

[MelCat]

I posted some tips here.

Great tips, for sure. Thanks for sharing them!

I was thinking about that later, 600ml might still be a bit too much for crystals to form.

The last extraction I did, over two years ago, was 500g of rue and that ended up in a 1 quart mason jar easily when it came time to manske. The key is to freebase the harmalas and once collected, add to a minimal amount of vinegar. Just enough to get everything dissolved. From there it's easy to figure out how much salt to use based on how many milliliters your solution is.

 

[Volrux]

"Hey there,
Well the jar is now in the fridge, by the way, I'm also extracting 500g of seeds. I reduced it to approximately 600 ml, and I added a little bit more salt during the process. The crystals have precipitated, but unfortunately they are not forming the beautiful big needles. But that was to be expected, I guess haha.
Well, I'm letting them rest for another half a day, and then I'll proceed with washing them again. Maybe in a later manske I will finally see the beauty of chemistry
Thanks again for all the support!"*


*The above text was whispered in my ear by a little bird

 

[Jees]

Before I manske, I go trough many acid-base steps, each time filtering the acid step until no catch anymore. Then I start poring like 5 times same acid tea trough same coffee filter over and over and start to catch again (dripping trough slowly is indicator). It is a very translucent bright yellow tea, before I manske.

Don't forget to fold the seams of the coffee filter in advance, very important!
I take fine white filters, dense paper, some brown are less fine where I live.

Happy trials

 

[Volrux]

Thank you for all the great tips Jees. I will definately do some more filtering before I will manske for the second time.

 

[MelCat]

I reduced it to approximately 600 ml, and I added a little bit more salt during the process. The crystals have precipitated, but unfortunately they are not forming the beautiful big needles.

Save the solution once you filter the needles out and reduce it down a lot more and allow it to cool again. With it being so much liquid, it could prevent some of the alks from falling out. You might end up with a bit of salt contamination but that's okay since you're going to base and manske again.

 

[Jees]

For the moment I'm not sure of the value of it, but first base-acid steps are done with HCL, and the latest ones with phosphoric acid. It seems to give a difference, switching the acid along the way, but I'm not 100% of the importance. For now, I think it does matter somehow, but unsure and dunno why if it does matter. Any info welcome.