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Quick and dirty (and effective) rue/harmala extraction. Options
 
SomewhatLost
#1 Posted : 1/13/2012 5:31:28 PM
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Hi all,

I've been experimenting with various rue extraction techniques and while many of the teks seem very well researched and effective, I couldn't help but think that many of them are unnecessarily complicated. I think I've got a technique now that is not only very easy to accomplish, but provides excellent yields as well. Here it is:

Materials needed: 2 large pots. A good amount of syrian rue. Water. Salt. Citric acid (or lemon juice or vinegar).

1) Add a large amount of rue to a large metal pot (the exact amount of rue isn't terribly important, I just find it much easier to work in large batches. The size of the pot should be enough that the rue doesn't come up to more than a third the height of it.)

2) Add enough water to the pot of rue so that the water level reaches about an inch above the rue.

3) Add around 1 gram of citric acid for every ounce of rue (lemon juice or vinegar would also work, of course, but vinegar smells awful and you'd need to account for it being very dilute).

4) Boil the rue for a good 40+ minutes.

5) Strain the rue water into a different pot and allow to boil down a bit.

6) Repeat steps 4 and 5 two more times, adding water each time.

7) By now, the rue should be pretty much spent and can be thrown away.

Cool Reduce the rue water to a simmer and begin to add plain ol' salt (non-iodized) to the rue water while stirring it.

9) Continue to add salt to the rue water until it becomes super saturated. When the water can no longer dissolve anymore salt, it should begin to accumulate at the bottom of the pot. I like to add about 7 grams of salt at a time and then stir for quite a bit. I do this until no more salt can be dissolved.

10) The rue water is then transferred to the fridge for an hour and then moved to the freezer.

11) Due to the high salt content of the water, it most likely won't freeze solid, but rather it should freeze in a kind of crystalline, chunky fashion.

12) When the water is semi frozen, you should see a clear separation between the dirty water and the harmalas at the bottom. I try to remove as much of the chunky ice as possible while leaving the harmalas and a bit of the slushy water behind. This can be done by hand (but be careful, frozen salt water is COLD)

13) Once you've got this harmala/slushy water mixture, you can then dry it in a few different manners:
A) Put it by a radiator or some other hot location until all the water is evaporated (this should provide a high yield, but there might be a bit of salt in the mixture.)
B) Put the mixture in a bowl and allow any ice crystals to melt. Then take about 6 paper towels and fold them into a thick, approximately 5"x5" square. Place this thick square of paper towels on top of the harmala/salt water mixture. The salt water should very quickly get sucked up into the paper towels while leaving the harmalas behind. Press the paper towels down to absorb as much of the salt water as possible. This should leave behind a mass of harmalas which is only slightly damp. The rest of the drying should go fairly quickly.


This is about the easiest method I can think of to extract harmalas and the yield seems to be pretty darned good. I got 13 grams of harmalas out of 224 grams of rue, that's ~6%, not bad at all for such a quick and dirty method. The harmalas seem to be very pure as well. I tasted a small bit and the bitterness completely overwhelmed any saltiness, I couldn't taste any salt at all. And the harmalas quickly turned my lips and tongue numb. I also really like using paper towels to absorb the salty water rather than attempting any kind of actual filtration which can be an incredible pain and very time consuming with harmalas. Almost none of the harmalas will get stuck to the paper towels and the salt water absorbs very quickly.

If anyone has any suggestions to make this easier or more efficient, please let me know.
 

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endlessness
#2 Posted : 1/13/2012 5:37:24 PM

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Thanks for sharing Smile Do you have some pictures of the final product?

Though Im very skeptical of testing purity by taste.. Did you at least bioassay them, with or without DMT?

You should get at least part of your harmalas (say, a gram), dissolve in water and add sodium carbonate to precipitate the cleaner freebase. That way you'll have a much more accurate dosage weight of your harmalas.
 
SomewhatLost
#3 Posted : 1/13/2012 6:18:14 PM
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endlessness wrote:
Thanks for sharing Smile Do you have some pictures of the final product?

Though Im very skeptical of testing purity by taste.. Did you at least bioassay them, with or without DMT?

You should get at least part of your harmalas (say, a gram), dissolve in water and add sodium carbonate to precipitate the cleaner freebase. That way you'll have a much more accurate dosage weight of your harmalas.


Hi Endlessness,

I don't have pictures right now, but I should be able to upload them tonight or tomorrow. Basically, it's just a somewhat darkish tan powder. As for a bioassay, I assume that means simply trying them out (sorry, I'm far from a chemist). Yes, I did try them out this morning. I took ~500mgs and got a rather pleasant sensation about 40 minutes later. I know you might think that this means that they're very dirty, but I seem to have a very high tolerance for harmalas and typically need to consume around 8 or so grams of rue to get full MAO inhibition. I got no nausea from this dose.

In the end, I think I'd rather leave my harmalas as is and take a larger than needed dose for inhibition than purify them further and risk dramatically reducing my yield. Once again, I'm far from a chemist and I don't even have so much as PH papers available right now. Aside from more accurate dosing, can you think of any other advantages to obtaining a freebase rather than an HCL? Do you find that the sodium carbonate precipitation doesn't reduce yield by much? Is it relatively easy to do without using PH papers? Thanks for your reply and thanks in advance if you happen to have some advice.
 
endlessness
#4 Posted : 1/13/2012 6:32:55 PM

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Hey Smile

Wow 8g rue for MAO inhibition seems like a lot! Personally I find that the MAO inhibition dosage is when I definitely feel 'something', like a light headedness, bit of sensitivity to light, maybe just a bit of dizzyness.. For me it would be around 3-4g rue for that.

I understand if you rather leave the harmalas as is, I mean, each one has their own way and thats just great Smile My only suggestion is, considering you have a yield of 13g, that spending just 1g for experimentation isnt a big part of your yield, and you can bioassay the resulting product and find for yourself if its worth the "trouble" (its no trouble at all, though), and the potential loss of yield.

As for how much yield you will lose, its very hard to say because it depends on purity of your initial product. At least some weight reduction is expected because harmalas in salt form are heavier than in freebase form, even if they are 100% pure (due to the extra HCl ion attached to each harmine/harmaline molecule). Also, one factor that we cant know beforehand is how much of your harmalas is harmine and how much is harmaline.. Harmaline is theoretically a bit water soluble even as a freebase, so freebasing might make you lose a small percentage of harmaline (less likely of harmine).

And regarding how you do it, just dissolve your harmala salts in a minimal amount of hot water, make a sodium carbonate saturated solution (dissolve as much sodium carbonate as you can in a certain amount of water, filter/decant away from excess sodium carb), and mixing the harmala solution with the sodium carb solution. As soon as you add, it will start cloudying/changing color.. Just keep adding till it stops changing color, and let it sit in the fridge for a couple of hours, then decant/filter your freebase alks... You dont need pH papers at all, and neither being a chemist (im neither one Smile )

Let us know if you try it out, im curious how much the weight reduces and how the resulting harmalas compare in terms of looks and bioassay results (and yeah bioassay is just trying them out, sorry for fancy wording there Very happy )
 
jamie
#5 Posted : 1/13/2012 6:46:12 PM

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I can guarantee you that those harmalas are not pure at all. What you did is basically just a maske tek except you froze it, that will give you a dirty product that might be like 50% pure I would think..

what you need to do is clean the final product somehow..a while ago I made a tek where I did a re-crystalization of harmine and harmaline(from manske) in just water..no vinegar and no salt. Just dissolve in the smallest ammount of water to dissolve them and bring the temperature down low enough so that the crystal precip out but so that the water does not freeze.

https://www.dmt-nexus.me...aspx?g=posts&t=25948
Long live the unwoke.
 
jamie
#6 Posted : 1/13/2012 6:51:09 PM

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"500mgs and got a rather pleasant sensation about 40 minutes later."

Even if you need 2 times the ammount of harmalas as most people, 500mg should give you more than a pleasant sensation. If you usually take 8g of harmalas I doubt that still gets near 500mg. If you really took 500mg of harmine/harmaline I think you would be in for a bit of an awakening.
Long live the unwoke.
 
SomewhatLost
#7 Posted : 1/13/2012 6:53:33 PM
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endlessness wrote:
Hey Smile

And regarding how you do it, just dissolve your harmala salts in a minimal amount of hot water, make a sodium carbonate saturated solution (dissolve as much sodium carbonate as you can in a certain amount of water, filter/decant away from excess sodium carb), and mixing the harmala solution with the sodium carb solution. As soon as you add, it will start cloudying/changing color.. Just keep adding till it stops changing color, and let it sit in the fridge for a couple of hours, then decant/filter your freebase alks... You dont need pH papers at all, and neither being a chemist (im neither one Smile )

Let us know if you try it out, im curious how much the weight reduces and how the resulting harmalas compare in terms of looks and bioassay results (and yeah bioassay is just trying them out, sorry for fancy wording there Very happy )


Yeah, I seem to have an abnormally high tolerance for the stuff. That, and I'm a pretty big guy. I've used ~5 grams of rue before and I'll definitely get some effects from DMT, but 8 grams ensures that I'll get the most out of it. I just really prefer to waste as little of the DMT as possible, especially when harmalas can be obtained so cheaply. When I take harmalas alone, I'll typically have around 500mgs, or 400mgs if it's pure harmaline and ~650mgs if it's harmine. That's just what I've found that works for me most effectively without causing much nausea or wasting too much.

I'll definitely give the freebase conversion a try, perhaps with a couple grams at first. I should be able to cook up some sodium carbonate fairly quickly.

As of late, I've taken to dosing both my harmalas and DMT in Jello, I think it's the perfect way to dose. I start by dissolving the DMT or harmalas in a very tiny bit of water and then adding some citric acid (the Persian market by my work has both Syrian Rue and citric acid for sale, it's incredibly convenient). I'll stir it a bit and let it sit for at least a half hour or so. Then I'll add a few ounces of water to a pot and bring it to a boil. I'll then add jello (preferably sugar free) until it's hard to dissolve any more. I'll turn off the range and let the thick jello mixture cool a bit and then I'll mix the jello mixture in with the water/citric acid/DMT or harmalas. This allows me to make the jello dose very small and because there's such a high jello to water ratio, the jello is very firm and easy to take without tasting much. Also, this method seems to kick things in much faster. It can sometimes take 2+ hours for DMT to kick in, but with this method, it tends to kick in around 45 minutes.

Thanks again for the advice.
 
SomewhatLost
#8 Posted : 1/13/2012 6:58:43 PM
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jamie wrote:
"500mgs and got a rather pleasant sensation about 40 minutes later."

Even if you need 2 times the ammount of harmalas as most people, 500mg should give you more than a pleasant sensation. If you usually take 8g of harmalas I doubt that still gets near 500mg. If you really took 500mg of harmine/harmaline I think you would be in for a bit of an awakening.


I was under the impression that most people required around 200mg of harmalas for potentiation, that's assuming the typical mix of harmine/harmaline in rue. Just to give you a frame of reference, I've taken 400mg of harmaline from an online vendor before and got a very similar feeling to the 500mg of harmalas I took this morning. I've taken 1gram+ doses of harmalas before and typically that just gives me a bit of nausea. For some reason, harmalas don't seem to have much of an effect with me.

My product might be dirty, but I really don't think it's anywhere close to 50%. I'd think that 75% would be closer to the lower limit as I'm fairly familiar with the effects of harmalas and 500mgs give me pretty similar effects to the 400mg I've taken of professionally extracted product.
 
SomewhatLost
#9 Posted : 1/13/2012 7:02:15 PM
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jamie wrote:
I can guarantee you that those harmalas are not pure at all. What you did is basically just a maske tek except you froze it, that will give you a dirty product that might be like 50% pure I would think..

what you need to do is clean the final product somehow..a while ago I made a tek where I did a re-crystalization of harmine and harmaline(from manske) in just water..no vinegar and no salt. Just dissolve in the smallest ammount of water to dissolve them and bring the temperature down low enough so that the crystal precip out but so that the water does not freeze.

https://www.dmt-nexus.me...aspx?g=posts&t=25948


Thanks for the advice, Jamie.

Quick question though. You mention that you should dissolve the harmalas in minimal water and then bring the temperature down low, but not to freezing. What would the problem be if it froze? For me, I find freezing harmala mixtures to be a great way of separating the harmalas from the liquid. Is there a reason that freezing is bad?
 
SnozzleBerry
#10 Posted : 1/13/2012 7:12:07 PM

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SomewhatLost wrote:
In the end, I think I'd rather leave my harmalas as is and take a larger than needed dose for inhibition than purify them further and risk dramatically reducing my yield.

Well, look at it like this. If you have a chocolate chip in a pile of sawdust and you wanted to taste the chocolate, sure, you could eat the whole thing, sawdust and all, or you could take the time to remove the chocolate chip from pile of sawdust. Now at this point, you might have a chocolate chip covered in sawdust, but it will give you significantly more chocolate for each bit of sawdust you have to eat. At a certain point, sure you may start to lose harmalas through further purification, but that would be akin to using a razor blade to scrape off the sawdust remnants on your chocolate and losing shavings of chocolate (point being you shouldn't really worry about losing alkaloids until you're at a relatively pure product anyway, imo).

You will probably reduce "yield" if you purify, I can't say if it will be dramatic or not, but the "yield" you lose should not be active alkaloids anyway, but unnecessary plant material.
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SomewhatLost
#11 Posted : 1/13/2012 7:18:38 PM
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SnozzleBerry wrote:
SomewhatLost wrote:
In the end, I think I'd rather leave my harmalas as is and take a larger than needed dose for inhibition than purify them further and risk dramatically reducing my yield.

Well, look at it like this. If you have a chocolate chip in a pile of sawdust and you wanted to taste the chocolate, sure, you could eat the whole thing, sawdust and all, or you could take the time to remove the chocolate chip from pile of sawdust. Now at this point, you might have a chocolate chip covered in sawdust, but it will give you significantly more chocolate for each bit of sawdust you have to eat. At a certain point, sure you may start to lose harmalas through further purification, but that would be akin to using a razor blade to scrape off the sawdust remnants on your chocolate and losing shavings of chocolate (point being you shouldn't really worry about losing alkaloids until you're at a relatively pure product anyway, imo).

You will probably reduce "yield" if you purify, I can't say if it will be dramatic or not, but the "yield" you lose should not be active alkaloids anyway, but unnecessary plant material.


Hi SnozzleBerry,

I appreciate the analogy, but I only think it would be apt if harmalas tasted like chocolate chips Smile. As I tend nowadays to consume my harmalas in jello without actually tasting them at all, I'm not so sure it would apply. Aside from being able to more accurately dose, are there any other reasons why a purification is necessary given my method of ingestion? My powder has no stickiness or residual rue smell. Aside from accuracy and the need to take less, is there anything else to gain by doing a purification?
 
SnozzleBerry
#12 Posted : 1/13/2012 7:27:14 PM

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Nope, not really, but as a hard head, I think consistency in dosing is pretty darn important for a variety of reasons. Hearing how much of this stuff you say you need to eat, I'd think that it would be of importance for all the reasons that go along with that, but, that's just me.

Also, why eat things you don't have to?
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SomewhatLost
#13 Posted : 1/13/2012 7:33:17 PM
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SnozzleBerry wrote:
Nope, not really, but as a hard head, I think consistency in dosing is pretty darn important for a variety of reasons. Hearing how much of this stuff you say you need to eat, I'd think that it would be of importance for all the reasons that go along with that, but, that's just me.

Also, why eat things you don't have to?


Well, I can generally get a pretty good idea of how much I need to take of this stuff to get full inhibition. For me, it tends to be around 500mg. And I really don't see much of a difference between having to have to eat 500mg of the stuff as opposed to 375mg. Either way, I'll be taking it in a tiny shot of jello, I definitely don't like to taste it Smile. As for the why not? Well, I've had poor success with purification techniques in the past. There have been times when I've lost a lot of my final product (either due to some obvious mistake or some unknown reason). I figure that if I can get a relatively pure product and a great yield using a simple technique, that works for me. If I intended to smoke a good portion of it, I'd probably do a clean-up/freebase conversion, but for oral ingestion, I don't see what's wrong with this method.
 
jamie
#14 Posted : 1/13/2012 7:33:21 PM

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SomewhatLost wrote:
jamie wrote:
I can guarantee you that those harmalas are not pure at all. What you did is basically just a maske tek except you froze it, that will give you a dirty product that might be like 50% pure I would think..

what you need to do is clean the final product somehow..a while ago I made a tek where I did a re-crystalization of harmine and harmaline(from manske) in just water..no vinegar and no salt. Just dissolve in the smallest ammount of water to dissolve them and bring the temperature down low enough so that the crystal precip out but so that the water does not freeze.

https://www.dmt-nexus.me...aspx?g=posts&t=25948


Thanks for the advice, Jamie.

Quick question though. You mention that you should dissolve the harmalas in minimal water and then bring the temperature down low, but not to freezing. What would the problem be if it froze? For me, I find freezing harmala mixtures to be a great way of separating the harmalas from the liquid. Is there a reason that freezing is bad?


You can freeze it..get it to the point where it is like a slushy..the harmalas will have dropped out of solution but you cant pour off the water and filter off the harmalas..so then stick it into the fridge for just enough time for the slushy to turn back into liquid and the harmalas should stay as precipitated crystals. Remember, you are not adding salt to the water this time, so it will freeze before salt water will, and if you use too much water the harmalas tend to stay in solution and not drop out-hence using only the bare minimum of hot water to dissolve them, then cooling.
Long live the unwoke.
 
SomewhatLost
#15 Posted : 1/13/2012 7:44:14 PM
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jamie wrote:


You can freeze it..get it to the point where it is like a slushy..the harmalas will have dropped out of solution but you cant pour off the water and filter off the harmalas..so then stick it into the fridge for just enough time for the slushy to turn back into liquid and the harmalas should stay as precipitated crystals. Remember, you are not adding salt to the water this time, so it will freeze before salt water will, and if you use too much water the harmalas tend to stay in solution and not drop out-hence using only the bare minimum of hot water to dissolve them, then cooling.



Thanks again for the advice, jamie. I think I'll be giving this a try. Does this result in a relatively pure product? Once again though, I need to ask, would it be a problem if I simply froze this minimal amount of water/harmalas and then removed it from the cup and separated the harmalas that way? This is the way that I've done it in the past and I've found that I'm able to lose a fair amount less of the product when compared to simply decanting.
 
Dozuki
#16 Posted : 1/13/2012 7:48:58 PM

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somewhatlost wrote:
is there anything else to gain by doing a purification?


Yes: More accurate dosage information for those who might use this method of extraction.

Without knowing the actual purity, then the initial dosage of such an extraction is also unknown. For your own personal use, this is fine. You know your procedure and how much of your extraction to use. Others are starting from scratch and your dosage seems to be much more than average.

Purification of these alkaloids is simple enough. If so yield is lost, it shouldn't be that big of a deal. Rue is high in alkaloids and cheap. The biggest gain here is accuracy.

My thinking is also this: if the extraction is only 75% pure then 25% of the yield is impurity. If it was cleaned up and you lost 26% then you have really only lost 1% of the alkaloids and have a more realistic yield amount. Again more accuracy.
 
SnozzleBerry
#17 Posted : 1/13/2012 7:54:05 PM

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SomewhatLost wrote:
Well, I can generally get a pretty good idea of how much I need to take of this stuff to get full inhibition. For me, it tends to be around 500mg. And I really don't see much of a difference between having to have to eat 500mg of the stuff as opposed to 375mg.

Right, but who knows if 500mg of batch A is the same as 500mg of batch B without purifying...seeds are variable in the %alks...that's some of what I was getting at regarding dosing.

I'm not knocking your method...if you find it works for you and you're happy with the results then by all means keep with it, just offering some thoughts Smile
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Dozuki
#18 Posted : 1/13/2012 7:56:32 PM

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Quote:
I'm not knocking your method...if you find it works for you and you're happy with the results then by all means keep with it, just offering some thoughts


Ditto!

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SomewhatLost
#19 Posted : 1/13/2012 8:02:36 PM
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Dozuki wrote:
somewhatlost wrote:
is there anything else to gain by doing a purification?


Yes: More accurate dosage information for those who might use this method of extraction.

Without knowing the actual purity, then the initial dosage of such an extraction is also unknown. For your own personal use, this is fine. You know your procedure and how much of your extraction to use. Others are starting from scratch and your dosage seems to be much more than average.

Purification of these alkaloids is simple enough. If so yield is lost, it shouldn't be that big of a deal. Rue is high in alkaloids and cheap. The biggest gain here is accuracy.

My thinking is also this: if the extraction is only 75% pure then 25% of the yield is impurity. If it was cleaned up and you lost 26% then you have really only lost 1% of the alkaloids and have a more realistic yield amount. Again more accuracy.


Thanks for the reply, Dozuki.

Yeah, I certainly can't say that this is entirely clean, but I'd be shocked if it's less than 75% pure. As I mentioned previously, I found the effects of the 500mg I took this morning to be remarkably similar to the effects of 400mg of ~95% pure harmaline I got from an online vendor. I guess I'd suggest that the user take approximately 30% more than they're accustomed to to get the same effect.

And yeah, I do think I'm going to purify my current batch. It's cheap enough and I've got a lot to work with. I understand that IDEALLY one shouldn't lose much of their yield which already wasn't garbage, but I've had bad luck in the past. Rather than say a 26% loss, in the past I've had occasions where I've lost 50% or more. I know you might think that this means that I've got a much dirtier product than I originally imagined, but once again, I'd be very surprised if it wasn't around 75% pure.

Regardless, I'm going to give it a try tonight, if for nothing more than practice. Thanks again.
 
SomewhatLost
#20 Posted : 1/13/2012 8:09:31 PM
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SnozzleBerry wrote:
SomewhatLost wrote:
Well, I can generally get a pretty good idea of how much I need to take of this stuff to get full inhibition. For me, it tends to be around 500mg. And I really don't see much of a difference between having to have to eat 500mg of the stuff as opposed to 375mg.

Right, but who knows if 500mg of batch A is the same as 500mg of batch B without purifying...seeds are variable in the %alks...that's some of what I was getting at regarding dosing.

I'm not knocking your method...if you find it works for you and you're happy with the results then by all means keep with it, just offering some thoughts Smile


I hear you and I definitely appreciate the information. The reason I joined the Nexus is so that I could get advice from the extremely knowledgeable people here and share my own experiences.

You (and others here) have certainly made your point. I'll be doing the purification and just hoping I don't have the kind of losses I've experienced in the past. I probably just need a bit of practice at it. Some of the methods I've heard described here seem rather simple. Perhaps I'll modify the tek so that after I go through the paper towel water absorption step, I add the still damp gob of harmalas into a small amount of warm water and then toss into the freezer for a bit.
 
 
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