TEK Manske Query

[kkRoxo]

Hi All

Hoping you might be able to help...

Been trying to do a rue extraction. Started with 100g seeds, boiled them down with vinegar, ran them through filters over a few days and did 2 manske cleanup steps. After the second one, there were big clean looking needles and the water colour was getting cleaner... All was going to plan! Wanted to do one more cleanup as apparently you should do 3 minimum, ideally.

However, after 24 hours, only a fine sediment and no crystals has been left... another manske was done just in case, but there's still the same issue.

Wondering if anyone has had this issue before and how you fixed it? The salt solution is at 10%. Pictures attached which hopefully show what's going on.

Thanks for any help you can give.

 

[blig-blug]

Has it been refrigerated?

 

[kkRoxo]

Has it been refrigerated?

Not at first and the crystals were growing fine. Once they stopped, it was put in the fridge, but nothing yet (been 24 hours).

 

[blig-blug]

I don't know what it could be, but you could try to reheat and add more NaCl to see if a higher concentration forces precipitation.

 

[kkRoxo]

I don't know what it could be, but you could try to reheat and add more NaCl to see if a higher concentration forces precipitation.

Yeah, increased the solution concentration and unfortunately still nothing...!

 

[blig-blug]

Just in case: are you sure the solution is acidic? That sediment you're getting looks similar to the freebase when it precipitates. Did you add some acid other than the initial vinegar when boiling?

 

[kkRoxo]

Just in case: are you sure the solution is acidic? That sediment you're getting looks similar to the freebase when it precipitates. Did you add some acid other than the initial vinegar when boiling?

Nothing acidic other than the initial vinegar was added when boiling. Would this still be possible to dry out and use? Or should a recovery of some sort be attempted, such as adding a base to it and trying again with the salt?

 

[blig-blug]

It could be that your water is basic enough to make some of it precipitate as freebase, but to be honest I'm not sure if that's possible. In general, when dissolving harmala HCl after the manske, it's a good idea to add some acid to make it dissolve better.

You could try adding a base to precipitate the freebase (and make sure that actually you do have alkaloids dissolved there) and then redissolve in acidic liquid and attempt the manske again.

And yes, if that sediment is harmala freebase (it should become yellow when dissolved in an acidic medium), it's perfectly possible to use it. Just dissolve it in some acidic liquid if you're going to consume it orally and you're all set. And if you're going to use it for changa, you should use the freebase form.

What tek were you following, if any? I think for your first extraction it's a good idea to follow a pre-existing tek so you are sure that you are doing everything right and see how it should look at each step, and then you can try your own variations.

 

[kkRoxo]

It could be that your water is basic enough to make some of it precipitate as freebase, but to be honest I'm not sure if that's possible. In general, when dissolving harmala HCl after the manske, it's a good idea to add some acid to make it dissolve better.

You could try adding a base to precipitate the freebase (and make sure that actually you do have alkaloids dissolved there) and then redissolve in acidic liquid and attempt the manske again.

And yes, if that sediment is harmala freebase (it should become yellow when dissolved in an acidic medium), it's perfectly possible to use it. Just dissolve it in some acidic liquid if you're going to consume it orally and you're all set. And if you're going to use it for changa, you should use the freebase form.

What tek were you following, if any? I think for your first extraction it's a good idea to follow a pre-existing tek so you are sure that you are doing everything right and see how it should look at each step, and then you can try your own variations.

Brilliant, thanks for this.

So, in order to recover this, what would your main recommendation be? Adding a base of sodium carbonate, then dissolving in an acidic liquid, then re-doing the Manske step?

I've been using the following guide...

Syrian Rue Extraction: How To Make An MAOI At Home - Entheogen Insight

This is an easy step-by-step guide to extracting Syrian Rue at home. A breakdown of all the supplies and tools needed for a success!

entheogeninsight.com

Their recommedation was 250g seeds. However, I reduced all amounts of 100g seeds, from which there is a 190ml solution now for the mankse step. Not sure what the ratios would be for adding a base and re-dissolving etc...

 

[blig-blug]

So, in order to recover this, what would your main recommendation be? Adding a base of sodium carbonate, then dissolving in an acidic liquid, then re-doing the Manske step?

That's what I would try if I were in a similar situation, as the only explanation that makes sense to me for what happened (other than having lost most of the harmalas) is that the bottom sediment is harmala freebase. Do you have pH strips? If you do, test the acidity of your solution: if it's even slightly acidic, it can't be harmala freebase and it may be very small crystals instead. It's still weird because your water is quite clear, and harmala HCl dissolved in water makes the water quite yellow. I hope you didn't lose the alkaloids at some previous step.

That guide looks about right (however I don't think you really need lye, and if you do use lye then you don't need sodium carbonate). For a first extraction, however, I recommend this one: TEK - Syrian Rue Seeds to Smokeable Freebase + Consumable HCL [Harmallama Tek] It includes no manske step except optionally at the end, and it's the one I used for my first extraction. Now I do something closer to this one, but without grinding the seeds: Harmalas Extraction and Separation Guide - DMT-Nexus Wiki

 

[kkRoxo]

That's what I would try if I were in a similar situation, as the only explanation that makes sense to me for what happened (other than having lost most of the harmalas) is that the bottom sediment is harmala freebase. Do you have pH strips? If you do, test the acidity of your solution: if it's even slightly acidic, it can't be harmala freebase and it may be very small crystals instead. It's still weird because your water is quite clear, and harmala HCl dissolved in water makes the water quite yellow. I hope you didn't lose the alkaloids at some previous step.

That guide looks about right (however I don't think you really need lye, and if you do use lye then you don't need sodium carbonate). For a first extraction, however, I recommend this one: TEK - Syrian Rue Seeds to Smokeable Freebase + Consumable HCL [Harmallama Tek] It includes no manske step except optionally at the end, and it's the one I used for my first extraction. Now I do something closer to this one, but without grinding the seeds: Harmalas Extraction and Separation Guide - DMT-Nexus Wiki

Brilliant, thanks for this, really helpful! Out of interest, how much sodium carbonate/water ratio would you add and then how much acidic liquid ratio, before moving to the manske step?

Does it need to leave them for 24 hour periods inbetweenen, like the guide has previously recommended?

 

[blig-blug]

how much sodium carbonate/water ratio would you add

Usually you should slowly add base until it suddenly changes color (due to the harmala alkaloids precipitating), and then a little bit more. It corresponds to a pH of around 11. You can add sodium carbonate directly or make a saturated solution first and then add that solution (sodium carbonate saturates water at about 22g / 100ml).

then how much acidic liquid ratio

There you don't need much vinegar as long as it makes the water acidic. I have seen teks that say it should be 50% vinegar and others that just say to add "a dash" of it. I like to add about 100ml vinegar per 500ml water just to be sure

Does it need to leave them for 24 hour periods inbetweenen, like the guide has previously recommended?

There's a tradeoff between convenience and losing yield there. You can wait as little as 2 hours and the losses will be quite low (but not insignificant). Many people leave it overnight, so around 8-12 hours. There's no harm in leaving it for longer, though. In my experience, at the early stages it's beneficial to leave it for a long time because the liquid is very viscous and the alkaloids precipitate slowly, whereas in the later stages, when the water is clear, you don't need more than a few hours.

 

[kkRoxo]

Usually you should slowly add base until it suddenly changes color (due to the harmala alkaloids precipitating), and then a little bit more. It corresponds to a pH of around 11. You can add sodium carbonate directly or make a saturated solution first and then add that solution (sodium carbonate saturates water at about 22g / 100ml).


There you don't need much vinegar as long as it makes the water acidic. I have seen teks that say it should be 50% vinegar and others that just say to add "a dash" of it. I like to add about 100ml vinegar per 500ml water just to be sure


There's a tradeoff between convenience and losing yield there. You can wait as little as 2 hours and the losses will be quite low (but not insignificant). Many people leave it overnight, so around 8-12 hours. There's no harm in leaving it for longer, though. In my experience, at the early stages it's beneficial to leave it for a long time because the liquid is very viscous and the alkaloids precipitate slowly, whereas in the later stages, when the water is clear, you don't need more than a few hours.

Will try adding a base and seeing what happens... fingers crossed!

 

[Varallo]

In addition to @blig-blug I Would suggest you use ammonia instead of sodium carbonate as this will help you create an clean precipitate that is just your alkaloids.
From there you can rather use it as is or convert to the salt from your after.

 

[kkRoxo]

So, here is what's left after adding the base... thoughts?

Does it look like scrap and re-try, or should the acidic solution be added?

 

[blig-blug]

If that's all that appeared after adding base, it likely means that that's all the alkaloids that are left. You likely lost them at some previous step, probably dissolving in some way the crystals in water that was then discarded.

or should the acidic solution be added

Just to clarify: if you were to do another acid-base cycle, you first would retrieve the freebase using a filter and then redissolve that in acidic water, not directly add acid to the base solution. I don't think it makes much sense to continue with the tiny amount you have left, but you can still filter it, let it dry and use it.

I recommend to follow one of the teks recommended above and take photos at each step. If at some step something weird or unexpected happens, you can share it here and someone will be able to help, particularly with the help of photos of the previous steps.

 

[kkRoxo]

If that's all that appeared after adding base, it likely means that that's all the alkaloids that are left. You likely lost them at some previous step, probably dissolving in some way the crystals in water that was then discarded.

Just to clarify: if you were to do another acid-base cycle, you first would retrieve the freebase using a filter and then redissolve that in acidic water, not directly add acid to the base solution. I don't think it makes much sense to continue with the tiny amount you have left, but you can still filter it, let it dry and use it.

I recommend to follow one of the teks recommended above and take photos at each step. If at some step something weird or unexpected happens, you can share it here and someone will be able to help, particularly with the help of photos of the previous steps.

Ahhh got you, thanks for all your help on this. Next time, the guide will be followed!

Out of interest, do you think that is freebase to be used once dried? Just concerned it might be a load of sodium bicarb...?

 

[blig-blug]

Out of interest, do you think that is freebase to be used once dried? Just concerned it might be a load of sodium bicarb...?

Well, it has some harmala freebase at least, given the color. If you are concerned that it has base (it could), you can always dissolve it in acidic water and do a manske. But it not may be worth it for such a small amount.

Did you use sodium bicarbonate? Sodium bicarbonate is not basic enough AFAIK, you should use sodium carbonate (or ammonia as @Varallo suggested). If you have sodium bicarbonate, you can convert it to sodium carbonate by baking it on a clean oven (there are instructions elsewhere in the Nexus).

 

[kkRoxo]

Well, it has some harmala freebase at least, given the color. If you are concerned that it has base (it could), you can always dissolve it in acidic water and do a manske. But it not may be worth it for such a small amount.

Did you use sodium bicarbonate? Sodium bicarbonate is not basic enough AFAIK, you should use sodium carbonate (or ammonia as @Varallo suggested). If you have sodium bicarbonate, you can convert it to sodium carbonate by baking it on a clean oven (there are instructions elsewhere in the Nexus).

Ah fair enough, thanks! Will probably just dry it out. Wasn't sure if that might make it trickier dosage wise. Though, by the sounds of things there won't be much.

Was using sodium carbonate, not bicarbonate, wrote the wrong thing!

 

[Varallo]

The easiest way to extract harmalas is to simmer the seeds material several times with a bit of vinegar. Collect the liquid each time, combine it, and store it in a large bottle in the refrigerator. Let it sit for a few days until the solution becomes completely clear. There is no need to filter or reduce your brew.

Carefully pour off the clear part, keep this, leaving any sediment behind. Then, add ammonia to the clear solution. This will cause the harmala alkaloids to precipitate out as freebase. This step will reduce the volume and save you the hassle of filtering significantly, and the alkaloids will settle.

Let this mixture stand for a couple of days without disturbing it. After settling, pour off the liquid on top (dispose). What remains at the bottom are your crude alkaloids.

Dissolve these again in a little bit of water with a bit of vinegar. This time, filter the solution properly to remove any insoluble material. Finally, add a saturated salt solution to help the alkaloids precipitate more cleanly.

You can easily extract large quantities of seeds without much effort.