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CWE workflow on grinded syrian rue & no filter problems. Options
 
Jees
#1 Posted : 8/3/2015 10:27:43 AM

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Beware not to break laws, be careful with acids and base, etc etc

If you have obtained grind seeds this might help you, but if you have whole seeds then before starting grinding you might check out the "aftermath" note.

This is just one take-on of many.
It's not about tec and chemistry, but workflow to avoid (at max) the typical problems that grinded syrian rue gives, namely filtering. To achieve that, the filtering is only done as late as possible when most plant gunk is already disposed of. This is where this workflow differs from "The TAO of rue extraction" and most others. We'll never filter the seeds powder here!

We will decant/siphoning off the liquid layers a la make a siphon-off jar. Not by tipping over and casting.

Because we gonna decant a lot, time will be the main ingredient to settle the matter in the jars, the plant matter and the FB. Each get a jar for that. Like 12 hours is typical for a settle period. So you start making when your stash is not run out with this method. Though this workflow goes over many days, the actual work is like 10 max 15 minutes per day.

Began this with 105gr seeds, dried in the oven at like 60 deg C (140 deg F) for like minimum 1 to better 2 hours, this makes grinding easier, and the weight gets like 5% less during drying, ending 100 gr of powder. Not overly fine to ease the process of grinding, more like coffee.

An optional freeze/thaw with the moistened powder is possible, I overlooked that possibility in this case.

Put powder in a jar, added just over 1 liter water + muriatic acid (32% here) making pH just above 1 is okay. Let this stand + shake often for like 4 days (in this case it was 2 weeks because of other projects taking time. If you had vinegar and wait for 14 days the mold has grown out of you windows, not so with HCL pH 1). So this is a cold water extraction.

Once this got settled, the acid top layer got siphoned of and into the FB-jar. Then pH was risen in FB jar with lye-water to 12 and topped up with water til full, this dilutes the dirt. The plant-jar got clean water, shaken, and it's pH went up to 1.3.

This is the starting situation like in the picture, settled FB and settled plant jar. pH 12 and 1.3. The workflow start actually from this point onward.

The reason why I post these pictures (more to come later) is to illustrate how clean it all gets before any filtering takes place. That is key. If you would try to filter any of these 2 jars at this point, a nightmare awaits, so we don't filter yet.
To be continued...
(the jars used are 1.6 liter each to completely full.)
Jees attached the following image(s):
jars.01.jpg (184kb) downloaded 678 time(s).
 

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TGO
#2 Posted : 8/4/2015 12:00:11 AM

Music is alive and in your soul. It can move you. It can carry you. It can make you cry! Make you laugh. Most importantly, it makes you feel! What is more important than that?

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Nice work, Jees! I'm looking forward to seeing the rest of it! I absolutely hate filtering rue! It is such a pain! Keep us posted! Smile Thumbs up
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Jees
#3 Posted : 8/4/2015 7:46:34 AM

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Thx TGO Pleased

So here's the routine:

With your siphon-off-jar, skim off the liquid pH 12 top layer of the left FB jar and discard that liquid. (It keeps your sewer piping system pretty clean, it dissolves all fats and soap scaling). Rinse the siphon-off jar with water.

Then siphon-off the still acid (at this point pH 1.3) liquid layer above the plant matter of the right jar, and poor it into the FB jar. So the rinsing water of the plant matter is transferred. This rinse-water is still rich in alkaloids to be retrieved when basing the FB jar *** .
What this does also is dissolve the FB into a salt form and this is something we want to happen. The first FB is really dirty brown. By re-dissolving it with the plant-matter-rinse-water it gets a chance to get rid of the dirt gradually. The first plant-rinse-water is strong acid enough, later rinse-water (being less acid) we might help a bit.

Then base the FB-jar with lye water again to pH 12
***: The alkaloids of the plant-rinse-water gets accumulated with the first FB now.
Fill FB jar with water til full so dirt gets diluted max.

Add tap water to the plant-matter-jar, shake it so to rinse the gunk, in this case we've now pH 1.5 here. In begin the pH rises slow, that's normal at low pH range, it's a logarithmic scale, later the pH rises will go more steep with each rinse.

When these two jars then get settled it looks like in the picture below.
This batch of seeds is dirty and I get a lot of brown, YMMV and get cleaner sooner.
We haven't touched a filter yet, and the plant matter actually will never be filtered.
Compared with first picture, already cleaning of both liquid and FB visible.
To be continued...

Jees attached the following image(s):
jars.02.jpg (50kb) downloaded 622 time(s).
 
Jees
#4 Posted : 8/5/2015 8:30:44 AM

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Routine repeated:

Skim off liquid base layer of FB jar + discard liquid.

Skim off plant rinse water layer pH 1.5 + transfer this liquid into FB pot.
This rinse water still carries alkaloids with it, which will collect in the FB jar.
The rinse water pH 1.5 was not acid strong enough to salt all the FB, the pH was like 6. Added 2 milliliter muriatic acid 32% to get it down at 2.5, so we helped a little bit. Then added lye water to reach 12, top up with water.
These salt/FB transitions are needed to clean the FB gradually. Evidence of this is the becoming whiter FB, and the dark base liquid taking the dirt.

Added new rinse tap water to the plant-matter pot, shake, pH is now 2.5

Let settle, then it looks like:
Jees attached the following image(s):
jars.03.jpg (50kb) downloaded 592 time(s).
 
Jees
#5 Posted : 8/7/2015 8:25:18 AM

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Another 2 rounds of washing/transferring etc..
There is little color change in the jars between the pics, so now we've rinsed the seed-matter enough to get all (or most) alkaloids out off it, after 5 times of rinsing it with water. The last rinse water was like pH 3.

The seed powder was never filtered Thumbs up
If something is difficult, don't do it if there is another way.

PS: the link in OP wasn't OK, is now edited.
Quote:
We will decant/siphoning off the liquid layers a la make a siphon-off jar. Not by tipping over and casting.
Jees attached the following image(s):
jars.04.jpg (50kb) downloaded 548 time(s).
jars.05.jpg (50kb) downloaded 549 time(s).
 
Jees
#6 Posted : 8/7/2015 8:42:29 AM

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The FB-jar base liquid got skimmed off and this liquid discarded, and then the last seed powder "skimmed off rinse water" added to the FB jar. Five ml of muricatic made it all salted again to pH 2.5.
You can do another acid/base transitions to clean up the alkaloids if you want, but i'll try to start filtering at this stage.
To be cont...
 
Jees
#7 Posted : 8/7/2015 10:51:12 AM

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This is the FB jar acidified to pH 2.5 , first picture.
A lot of gunk at the bottom that does not serve us, prolly own to this kind of workflow
I would not suggest to filter right away, would be hard, but to let settle first like in the pic.

The top liquid layer gets skimmed off with your trusty siphon-jar and liquid run trough a coffee filter, this takes some time like 30 - 45 minutes, this is the hardest filter-job in this process and thus very doable compared to filtering powdered seeds which is more like un-filterable with coffee filters.
I do not but you can filter 50% volume in one and 50% in another coffee filter and then things take only 15 minutes. But actually I like to let it drip slow as the outcome is much more clear.

The bottom gunk layer gets it's own coffee filter and take just as much time as the above.
In second picture the left one filters the top liquid layer, the right one the bottom gunk.
Jees attached the following image(s):
fbja.jpg (50kb) downloaded 519 time(s).
filt.01.jpg (50kb) downloaded 516 time(s).
 
TGO
#8 Posted : 8/7/2015 4:09:31 PM

Music is alive and in your soul. It can move you. It can carry you. It can make you cry! Make you laugh. Most importantly, it makes you feel! What is more important than that?

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Damn Jees! You have been busy! Big grin

I'm loving watching this unfold as it seems very straightforward! I think I will be working with this method next time I do a Rue extraction. I have 800 grams just sitting around so... Anyway, great work as always!
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Jees
#9 Posted : 8/8/2015 8:07:41 AM

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Thanks for sheering up Very happy

Maybe with the former step:
Jees wrote:
This is the FB jar acidified to pH 2.5 , first picture.
A lot of gunk at the bottom that does not serve us...
maybe I was little too fast. There might have been some more goodies in the bottom gunk. I've seen before that FB flocculation might take some time to dissolve, even in acid water. So next time I will leave it like 10 hours in the acid water and shake once'n a while. Then let it settle.
Dunno if I lost some yield in this step, I let in only like 1 hour total in the acid water (I've only stirred once and let then settle).
Any thought on this welcome.

* * *

The picture below is the filtered acid liquid, basified with lye water to pH 12 and settled overnight. It's very fluffy and it let itself filter very easily. The first no-plant-gunk real FB as a product. This seed is very hard to get white off FB, very different from other seed. Several AB transitions can't better it.

From here, all the rest is nothing new as a workflow, but I'll post some steps anyway.
Mission accomplished: we achieved to beat the grinded seed Thumbs up
Jees attached the following image(s):
ffb.jpg (40kb) downloaded 732 time(s).
 
Jees
#10 Posted : 8/8/2015 10:18:37 AM

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Lining up for the first manske:
So I skimmed off the top base layer with the siphon jar, and coffee filtered the FB bottom layer, this goes really fluent. Discard base liquid.

While the coffee filter is still very wet (nothing dried):
Now to retrieve the FB out of the coffee filter I don't scrape it out of it. I tear the filter open and flush the FB out with a mix of water + vinegar, see attached .avi file.
The liquid becomes dark because the FB salts immediately on the vinegar.
 
Jees
#11 Posted : 8/9/2015 9:15:32 AM

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Now if you change acid like in this case I've always used muriatic (a strong acid) toward a lesser strong acid, here vinegar in the above post, then it's a good practice to filter again before adding the NaCl salt. It seems that going toward a lesser strong acid creates some particles that got liquid with the strong acid. So coffee filter this stage, I got some considerable solids catch very well worth the only little effort.

For making needles first time here: worked with 0,5 liter total and 75 gr salt (so 15gr/100ml). pH was like 3,5
When the solution is still warm I always let it go trough a coffee filter once more, sometimes the added salt makes solid things that get caught in the filter at this stage.

To be cont....
 
Jees
#12 Posted : 8/12/2015 2:19:02 PM

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After 2 manskes, the loot is in,
6.36 gr of rueHCL
Out of 105 gr seed this means 6 % yield rueHCL.
This is my poorest batch of rue so far, normally I get even 1% more.

No cooking, no filtering problems.

This was 14 days soaked rue seed powder, regular shaking.
If I let it soak for 4 days, then yield drop to 5 %.

Happy days
Pleased
Jees attached the following image(s):
Loot.jpg (164kb) downloaded 444 time(s).
 
TGO
#13 Posted : 8/12/2015 2:45:36 PM

Music is alive and in your soul. It can move you. It can carry you. It can make you cry! Make you laugh. Most importantly, it makes you feel! What is more important than that?

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Amazing results, Jees! Well done!

Thumbs up Thumbs up

Smile
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Jees
#14 Posted : 8/12/2015 3:32:06 PM

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The Grateful One wrote:
Amazing results, Jees! Well done!

Thumbs up Thumbs up

Smile

Thanks for sticking around brother TGO.
I have no urge to display works but every time I saw a post that grinded rue is a pain-in-the-@ss I wanted to scream Not-True Laughing . So I felt responsible in a way to prove something. Also getting more out of resources is form of respect and powdered does comply with this, no cooking too. The extra time needed for the several settlings creates a bound. Then each day a 10 minute job only for repeating the routine. After the soak-period I had a 10 days extraction period, if in a hurry one could settle-time less and do in half, but I really was in no hurry. Life is good when there is still some stash to run on Pleased
 
Jees
#15 Posted : 9/14/2015 5:20:16 AM

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Aftermath:

this far I've had no better yields than with grind seeds. Whole seeds boiling and simple straining always had less yield.

Yet by applying freeze/thaws + force to empty whole seeds the balance seems to tip in favor of not grinding anymore:
https://www.dmt-nexus.me...aspx?g=posts&t=66485

So if you had readily grind seeds, you can follow the washing-style presented here, but since squeezing whole seeds is very effective I won't start to grind on purpose.

I haven't checked what freeze/thaws can add to the grind-workflow, but I see not much use trying it out just for the sake of it.
 
Jees
#16 Posted : 11/18/2017 9:00:28 PM

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After aftermath:

this thread illustrates that even the most difficult filter-job for SR can be bypassed. People should not have filter problems.

From there I moved to squeezed whole seeds. (Sakkadelic style)

From there I moved to pressure potting whole seeds.
https://www.dmt-nexus.me...&m=822711#post822711

Syrian Rue is easy, if you have the work arounds.
Thumbs up

 
null24
#17 Posted : 11/19/2017 5:26:12 PM

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Thank you thank you thank you.

I've wanted to do this for some time but became daunted at the seeming difficulty.

My experiments with rue therefore have only been smoking seeds, or failures at teas.

I'll try this....
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
pitubo
#18 Posted : 11/19/2017 8:34:52 PM

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I have done an extraction on ground rue seeds only once. Already the grinding itself is a nuisance. My coffee grinder couldn't break down almost a third of the seeds, no matter how long I tried. And then the sludge that results from boiling the rue powder is pretty much unworkable after that.

Boiling whole seeds is the only reasonable way IMHO.
 
Jees
#19 Posted : 11/19/2017 9:57:18 PM

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pitubo wrote:
Boiling whole seeds is the only reasonable way IMHO.
Indeed.

Only good way to grind rue seeds is a drying session in the oven first.
Lost like 5 % of weight in the process.
Cant recall what I did, maybe 30 mins at 150 deg C? Just guessing.

Now it's pressure pot swings on my stove, multiple of those swings in a wash.
Water in and out da seeds with each swing ...
All you need and no hassle Cool
 
pitubo
#20 Posted : 11/20/2017 12:16:31 AM

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It's not strictly true that I performed only one extraction ever on ground rue seeds. I made another extract of a different kind from ground rue seeds: a butane extract. I will post about that some other time, in a different topic..
 
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