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Filtering Trouble

onward33

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Hi all - got to step 10 of this tek and using a single coffee filter and it just stops up. I can't seem to get things moving. This is my 2nd attempt, I used sodium bicarbonate the first time and this time tried lye to hopefully make filtering easier but it's the same issue. Any tips, or hacks? Right now, after things became 100% plugged up again, I just put my solution back together and it's now sitting in my fridge and is settled with what I think is all the freebase sitting at the bottom of the mason jar. Thank you!
 
I don't know what you could do to salvage your current extraction, but for the next time, don't grind the seeds. Instead, do several boils and then reduce the combined water from the boils. Then you won't have filtering issues, and the need to filter at all will be greatly reduced.
 
Vacuum filtration with a vacuum flask, Buchner funnel, and proper filter papers will make this a whole lot easier. You can skip an electrical/mechanical vacuum pump and just use a water aspirator pump.

Alternatively, from where you're at without getting any new gear you could just let the harmala freebase settle, decant as much liquid off as you want or feel comfortable removing, and then pour the rest of the solution and precipitate into your filter, resulting in far less liquid needing to go through the filter. Then you just need to wait.

Another option would be to remove as much liquid as possible (via decanting) and then re-acidify the freebase precipitates while they're still in solution. Then allow the acidified solution to rest before filtering (to let the gunk settle). After filtering, basify your solution again and the freebase precipitates should be easier to collect. You could do a manske after you filter the acidified solution and before you base it again, but the additional a/b alone should help clean things up a good bit.

You can also just use a ton of coffee filters (one after another), but that's also easier once the solution is a bit cleaner.

With all that said, I really can't recommend a proper vacuum filtration set strongly enough for harmala extraction, it makes worlds of difference.
 
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Vacuum filtration with a vacuum flask, Buchner funnel, and proper filter papers will make this a whole lot easier. You can skip an electrical/mechanical vacuum pump and just use a water aspirator pump.

Alternatively, from where you're at without getting any new gear you could just let the harmala freebase settle, decant as much liquid off as you want or feel comfortable removing, and then pour the rest of the solution and precipitate into your filter, resulting in far less liquid needing to go through the filter. Then you just need to wait.

Another option would be to remove as much liquid as possible (via decanting) and then re-acidify the freebase precipitates while they're still in solution. Then allow the acidified solution to rest before filtering (to let the gunk settle). After filtering, basify your solution again and the freebase precipitates should be easier to collect. You could do a manske after you filter the acidified solution and before you base it again, but the additional a/b alone should help clean things up a good bit.

You can also just use a ton of coffee filters (one after another), but that's also easier once the solution is a bit cleaner.

With all that said, I really can't recommend a proper vacuum filtration set strongly enough for harmala extraction, it makes worlds of difference.
I reacidified, filtered, rebased, and its settling now. Definitely lighter color layer above the settling precips. I've searched in the past and tried again just now, but what is a manske exactly? Can you explain or point me to a thread that explains it? Thanks again.
 
Awesome! Sounds like you're making good progress :)

Here's some practical manske info: The Tao of Rue Extraction - DMT-Nexus Wiki

It's an extraction route (or part thereof) that yields pretty harmala hcl crystals. I suggested it as an optional step after re-acidifying because precipitating the hcl crystals should leave additional unwanted plant matter in solution, further purifying your resulting product. However repeating a/b is also pretty effective (as it sounds like you've found).

Richard Manske was the Canadian chemist who first synthesized DMT and characterized and synthesized harmine and harmaline, and developed this extraction technique, which bears his name.

Do let us know how you go!
 
I reacidified, filtered, rebased, and its settling now. Definitely lighter color layer above the settling precips. I've searched in the past and tried again just now, but what is a manske exactly? Can you explain or point me to a thread that explains it? Thanks again.
The basic principle is to almost saturate a hot acidic harmala solution with salt, as it cools down and the solubility of both harmalas and salt reduce, the salt will push the harmalas out as it is much more readily soluble in water. You endup with beautiful long harmala hcl needles. This process helps further purify the product and the resulting harmala hcl is more shelf stable than the freebase. But when you collect the wet needles and dry them there will be some salt contamination which is fine but makes dosing inaccurate. So it's better to use less salt (it will still work) and remove as much as possible of the water before drying, if your plan to convert to freebase anyway, then it doesn't matter much.

Regarding filtering, it's best to work with whole seeds and do multiple A/B cycles, water washes, and manske before any filtration. You just filter at the last acidic phase.
 
The basic principle is to almost saturate a hot acidic harmala solution with salt, as it cools down and the solubility of both harmalas and salt reduce, the salt will push the harmalas out as it is much more readily soluble in water. You endup with beautiful long harmala hcl needles. This process helps further purify the product and the resulting harmala hcl is more shelf stable than the freebase. But when you collect the wet needles and dry them there will be some salt contamination which is fine but makes dosing inaccurate. So it's better to use less salt (it will still work) and remove as much as possible of the water before drying, if your plan to convert to freebase anyway, then it doesn't matter much.

Regarding filtering, it's best to work with whole seeds and do multiple A/B cycles, water washes, and manske before any filtration. You just filter at the last acidic phase.
Hey Sakkadelic,

I keep seeing people mentioning your tek but I’m not sure which tek they are referring to?

Would you be so kind as to point me in the right direction 😊

Thank you!
 
Thanks @blig-blug for linking it
@deeMte check out this one too
I really should rewrite that first tek sometime, it's from the first times I did any extraction, here's the main points.

1 - prepping the tea: starting with washed (removing any dirt/powders) whole seeds, whether short 5 min microwave boils or long 30 min stove top boils and squeezing the liquid out of the seeds between boils, this is the most fundamental point, to make a good tea, the rest is simple imo. freeze/thaw cycles and mashing the seeds between boils help to make things easier, as long as we're not making fine powders that make filtering hard.

2 - base and let the harmala freebase settle, decant the water and do a few water washes until the liquid looks cleaner. this gets rid of most of the impurities without filtering.

3 - acidify, there will be stuff that won't dissolve, don't try adding more acid to dissolve them, keep the volume minimal, let settle and filter with loose cotton and only dump the lower portion with the undissolved stuff into the filter at the end.

4 - redo basification + water washes and acidification and filtering until satisfied with purity (liquids looking crystal clear)

5 - do 1 manske step. dry and collect product if harmalas hcl is desired

6 - 1 final basification with minimal base, 2-3 water washes, dry and collect product if freebase harmala is desired.
 
Thanks @blig-blug for linking it
@deeMte check out this one too
I really should rewrite that first tek sometime, it's from the first times I did any extraction, here's the main points.

1 - prepping the tea: starting with washed (removing any dirt/powders) whole seeds, whether short 5 min microwave boils or long 30 min stove top boils and squeezing the liquid out of the seeds between boils, this is the most fundamental point, to make a good tea, the rest is simple imo. freeze/thaw cycles and mashing the seeds between boils help to make things easier, as long as we're not making fine powders that make filtering hard.

2 - base and let the harmala freebase settle, decant the water and do a few water washes until the liquid looks cleaner. this gets rid of most of the impurities without filtering.

3 - acidify, there will be stuff that won't dissolve, don't try adding more acid to dissolve them, keep the volume minimal, let settle and filter with loose cotton and only dump the lower portion with the undissolved stuff into the filter at the end.

4 - redo basification + water washes and acidification and filtering until satisfied with purity (liquids looking crystal clear)

5 - do 1 manske step. dry and collect product if harmalas hcl is desired

6 - 1 final basification with minimal base, 2-3 water washes, dry and collect product if freebase harmala is desired.

Awesome, thanks for linking. I’m going to try one of your teks next time as they seem straightforward.

At the moment I’ve followed BountyBotanicals tek and have completed the first manske. I’m hoping you could help me with what’s next 🙏

You’ll see in my pic 2 jars, the one on the right is the manske result which I’ve re-based several hours ago. This hasn’t had any water washes as it’s not part of that tek. Should I just switch to your Point 2 above now?

Also, the jar on the left is what went through the coffee filter after that first manske. It looks like more alkaloids sitting at the bottom but I’m not sure? Should I decant that jar and acidify it again or is it just trash?

Sorry to be a pain and thank you for your help!
 

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Awesome, thanks for linking. I’m going to try one of your teks next time as they seem straightforward.

At the moment I’ve followed BountyBotanicals tek and have completed the first manske. I’m hoping you could help me with what’s next 🙏

You’ll see in my pic 2 jars, the one on the right is the manske result which I’ve re-based several hours ago. This hasn’t had any water washes as it’s not part of that tek. Should I just switch to your Point 2 above now?

Also, the jar on the left is what went through the coffee filter after that first manske. It looks like more alkaloids sitting at the bottom but I’m not sure? Should I decant that jar and acidify it again or is it just trash?

Sorry to be a pain and thank you for your help!
oh that's looking pretty good!

for the jar on the right there's no need to clean it further, you can go ahead and decant, do 2 water washes (top with distilled water, settle, decant), on the last decant remove as much as possible of the water then put in a wide dish and dry it with a fan. I like to put it in the fridge during settling, I think the fridge vibrations help it settle better.

water washes are not just to further purify it but also to minimize any base residue in the final harmala freebase product so they're highly recommended after the final basification.

for the jar on the left (i'm assuming you basified the manske liquid) it's most likely more harmalas alks, iirc there's usually at least 5% alks left behind after manske. there's a strange thing that sometimes happen and results in blobs that refuse to settle, they look like harmalas but I never figured out what they are. your case looks more like haramala alks so you should try and recover it. so yes, decant, acidify, filter and discard the undissolved stuff, base and continue like the other jar.

good luck and you're most welcome :)
 
You’re a superstar, thank you so much for your detailed reply.

I’m going to go ahead and follow your advice and hopefully I won’t have to drink rue tea ever again 🤞😂
 
oh that's looking pretty good!

for the jar on the right there's no need to clean it further, you can go ahead and decant, do 2 water washes (top with distilled water, settle, decant), on the last decant remove as much as possible of the water then put in a wide dish and dry it with a fan. I like to put it in the fridge during settling, I think the fridge vibrations help it settle better.

water washes are not just to further purify it but also to minimize any base residue in the final harmala freebase product so they're highly recommended after the final basification.

for the jar on the left (i'm assuming you basified the manske liquid) it's most likely more harmalas alks, iirc there's usually at least 5% alks left behind after manske. there's a strange thing that sometimes happen and results in blobs that refuse to settle, they look like harmalas but I never figured out what they are. your case looks more like haramala alks so you should try and recover it. so yes, decant, acidify, filter and discard the undissolved stuff, base and continue like the other jar.

good luck and you're most welcome :)


Whoa, I just re-acidified the jar on the left then based it. I can’t sit the jar on my fridge so I sat it on my phone with a vibrating app going for 10 minutes. Insta-separation 🎉
 

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That's awesome! On the final wash let it settle longer even without vibration so that they compact and you can decant more of the water.

Another tip is to let the jar sit with small inclination, just raise it 1 cm from one side, like this the harmalas will accumulate towards one side, and then you can decant the water from that side, like this you can pour more of the water before the harmalas get disturbed. If you do that make sure it's well secured and can't easily fall off.
 
That's awesome! On the final wash let it settle longer even without vibration so that they compact and you can decant more of the water.

Another tip is to let the jar sit with small inclination, just raise it 1 cm from one side, like this the harmalas will accumulate towards one side, and then you can decant the water from that side, like this you can pour more of the water before the harmalas get disturbed. If you do that make sure it's well secured and can't easily fall off.
Ah that sounds like a good tip, I shall let them rest inclined. I’ll also start brewing one last tea for today so I don’t rush the last couple of washes and the drying 😂

A typical Pyrex baking dish like we use to precip dmt would be ideal for drying it out yeah?
 
Ah that sounds like a good tip, I shall let them rest inclined. I’ll also start brewing one last tea for today so I don’t rush the last couple of washes and the drying 😂

A typical Pyrex baking dish like we use to precip dmt would be ideal for drying it out yeah?
Yeah that'll work, the wider the better. It'll probably take 12-24 hrs to fully dry.

Do you take rue regularly?
 
Yeah that'll work, the wider the better. It'll probably take 12-24 hrs to fully dry.

Do you take rue regularly?

Cool.
Yep, every day for the last couple of months. I just boil 5g and take half of it, and I’ll top up if need be.

This is why I need to try the freebase because the tea is rancid lol
 
Is
Thanks @blig-blug for linking it
@deeMte check out this one too
I really should rewrite that first tek sometime, it's from the first times I did any extraction, here's the main points.

1 - prepping the tea: starting with washed (removing any dirt/powders) whole seeds, whether short 5 min microwave boils or long 30 min stove top boils and squeezing the liquid out of the seeds between boils, this is the most fundamental point, to make a good tea, the rest is simple imo. freeze/thaw cycles and mashing the seeds between boils help to make things easier, as long as we're not making fine powders that make filtering hard.

2 - base and let the harmala freebase settle, decant the water and do a few water washes until the liquid looks cleaner. this gets rid of most of the impurities without filtering.

3 - acidify, there will be stuff that won't dissolve, don't try adding more acid to dissolve them, keep the volume minimal, let settle and filter with loose cotton and only dump the lower portion with the undissolved stuff into the filter at the end.

4 - redo basification + water washes and acidification and filtering until satisfied with purity (liquids looking crystal clear)

5 - do 1 manske step. dry and collect product if harmalas hcl is desired

6 - 1 final basification with minimal base, 2-3 water washes, dry and collect product if freebase harmala is desired.
Do people typically use freebase or hcl for changa? My sense was freebase but wanted to be sure. Thanks for helping us noobs, I feel like there's less hostility towards newer folks on the nexus forum than basically anywhere else Ive posted on the internet. =) I edited out my 2nd question since I re-read your response below and saw my answer.
 
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