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1st extraction (Q21Q21 tek) -Great yields? Options
 
VoyagerGrey
#1 Posted : 9/4/2023 2:59:41 AM
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This is part 2 of a fictional story about someone called "Myself" who is, of course, not myself at all, but for convenience sake I shall proceed in the 1st person. For those who care, here is Part1. For those who don't, It ends with me, sitting on a stack of screen shots of hand written notes and all the necessary supplies to do an MHRB extraction, and an absent guide, coming here for answers.

TLDR / take aways:

I *think* I got 2.5g of spice out of 100g of MHRB. Maybe. If so, that would seem to indicate either a really potent batch of MHRB powder, OR, that there are a few additional steps possibly worth taking to maximize yields from the Q21Q21 Vinegar/Lime/Limonene tek. My process and findings are detailed below.
Edit (Sep 4): After weighing left over chalky residue from a vaporized dose which I now believe to be calcium carbonate, the byproduct of decomposition of calcium acetate present in my tincture, and subtracting that from my expected dose, I now believe my total yield to be about 55% of my initial estimate, so something like 1.375g

A bit of searching later I discovered that the hand written notes I was following were pretty much verbatim Q21Q21's Vinegar/Lime A/B Extraction Tek. So, I followed the process, almost to the letter, with a few minor changes as noted below, and just wanted to report what I did and what resulted. Spoiler alert- success! ( I think)

As per the advice I was given by my absent guide, I used Tek 1/ The Jimjam Party. I wanted to end up with Jimjam acetate, which is my only previous reference point, and I didn't want to f**k around with noxious/flamable fumes in my kitchen. Vamos.

Starting with 100g MHRB, the tek was followed to the letter with the following exceptions:

*It took a bit more lime to achieve what I think is the right consistency. Recipe called for 150g lime per 100 MHRB "but more won't hurt". So I ended up using 200g of lime to soak up enough liquid.

*Wasn't clear to me from the write up if I was to wait the 6-8 hours before or after drying the mix to a "crumbly" consistency, so I let it sit overnight, then spread on a SS baking tray and used a dehydrator (not oven. Lower temp, constant built in fan going) to get it to a pretty dry, crumbly texture, which only took about an hour, as opposed to the 3-5 days I was told it might take to evaporate on open air.

*It took more Limonene than suggested to cover my sludge. Way more. The tek suggests up to 200ml limonene for 100g MHRB. I ended up having to pour in 500ml to saturate the mixture and have a layer of clear solvent on top.

*Did 3 solvent pulls each followed by a vinegar wash at 0,24,48 hrs as suggested, except on 3rd solvent pull, I wanted to recover as much solvent as possible so piled my wet sludge into some cheese cloth and squeezed the living bejeezus out of it. All told I recovered 400ml of solvent (out of 500ml used)

*After this 3rd pull, I did 3 vinegar washes of the solvent until on the third one I couldn't see any noticeable colour in the vinegar. To get a complete and clean separation, I picked up most of the vinegar with a glass turkey baster, and then put the jar in the freezer. The vinegar freezes, the limonene doesn't (unless your freezer goes to -75c). Pour off the limo and store for future use, wipe down the jar and frozen vinegar with a paper towel and then remove the ice and add to the vinegar jar. Voila. Full separation without picking up any solvent.

The idea for multiple vinegar washes and freezer separation came from a mescaline extraction tek *somewhere* on this forum (but I can't remember where) that seems essentially identical to the Q21Q21 tek. I came across it searching for answers because I was worried about a slight film/bubbles that were forming in the jar where the vinegar contacts the solvent. Did I use some non solvent safe plastic that has ended up in my brew? I now believe that was very fine plant matter particulates causing a bit of an emulsion.

At any rate- I think the multiple washes and freezer step were worth it- I ended up with two 250ml jars of collected vinegar- one contained the combined vinegar from the first 2 pulls/washes, and the other had the results from the 3 washes on the 3rd and final pull. This may not be a conclusive indicator, but both jars contained roughly as much vinegar, and my "3rd pull" jar had as much colour or slightly darker than the other.

Now to evaporate and reduce to a tincture...
Done in a small pot on the stove top until I was left with pretty much exactly 14 ml of reddish liquid, measured quite precisely by picking up with a syringe and transferring into a dropper bottle.

At this point I don't know, and was not able to find out what my MIA guide usually did to measure the concentration. Being rather precision oriented myself, and wanting an objective measure of my yield independent of my vaporization technique, which no doubt would present it's own learning curve (there will be another post on that VV soon, I have some questions...)I opted for the "Quantitative Method"

I evaporated 10 drops on a glass coaster heated on the stove top to 110c (verified by meat thermometer) until dry/ no detectable vinegar fumes. interestingly, I did not end up with so much of a "goo" as expected, but more of a waxy substance with a dark amber colour. Anything more liquid than that really still smelled of vinegar. Diligently scraped this up onto a clean, previously weighed razor blade, and weighed in at 45mg.

Some (litteral) back of the envelope calculations indicated that I had produced 25g of Jimjam out of my 100g of MHRB powder! That's not only the most phenomenal yield anyone has ever reported, it's also a Christmas miracle, in that a bottle containing roughly 14g of liquid can hold 25g of magic! A bit of head scratching later I figured out that I was not in posession of a hyperspace tincture bottle, I had just lost a decimal. That's 45 mg per 10 drops, not per drop. Or 4.5mg per drop.

Interesting point- The internet will tell you that the unit of measure "drop" equals 0.05ml. However, with several attempts at measuring with a syringe and the dropper from my bottle, I clocked an average of 20 drops per 0.5 ml. or 0.025ml/drop, and that's the figure I used to calculate the total Jimjam content of my 14ml of tincture at 2.52g.

That's still a phenomenal yield, *if* I'm correct. I have some doubts due to the test evaporation becoming more of a solid/ wax than a goo, which is just not what I expected. I *did* vaporize this 45mg of waxy goo over several attempts with varying success, and one attempt did send me deep into the cosmic waiting room but only for about 5 minutes... There's no doubt I'm having some issues with vaporization though, and there will be another post for that. More test flight will be occuring in short order, and I'll be sure to report back.

Thoughts? Prayers? Hopes? Your input is welcome. Please be kind to a rookie pilot. Thumbs up

Mush Love!

 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
downwardsfromzero
#2 Posted : 9/4/2023 9:32:23 PM

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While a 2.5% yield from MHRB is not wholly unheard of, I rather suspect that the acetate decomposition does not run to completion. This may have inflated your yield by some small amount, although there may indeed be some amount of contaminants such as calcium acetate in particular increasing the apparent mass as well.

Thus the question: did you let the limonene stand so that any fine particulates had time to settle out and get removed by decanting the limonene off into a clean vessel before doing the vinegar washes? If there is lime in the limonene you will get calcium acetate in the end product. One easy presumptive test for it is to add isopropanol, which forms a gel with calcium acetate (and this gel is used nowadays for bbq lighting paste and similar purposes). Ethanol (everclear) may also work, iirc.

What form - liquid or solid - did the end product of the thermal acetate decomposition have while it was still hot?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
VoyagerGrey
#3 Posted : 9/5/2023 12:23:13 AM
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downwardsfromzero wrote:
While a 2.5% yield from MHRB is not wholly unheard of, I rather suspect that the acetate decomposition does not run to completion. This may have inflated your yield by some small amount, although there may indeed be some amount of contaminants such as calcium acetate in particular increasing the apparent mass as well.

Thus the question: did you let the limonene stand so that any fine particulates had time to settle out and get removed by decanting the limonene off into a clean vessel before doing the vinegar washes? If there is lime in the limonene you will get calcium acetate in the end product. One easy presumptive test for it is to add isopropanol, which forms a gel with calcium acetate (and this gel is used nowadays for bbq lighting paste and similar purposes). Ethanol (everclear) may also work, iirc.

What form - liquid or solid - did the end product of the thermal acetate decomposition have while it was still hot?


I'm more inclined to believe there's room for improvement rather than my first extraction being absolute wizardry...Laughing There's just a lot of factors to consider and more trials are needed before drawing conclusions. The test you propose should be done on what material? At what stage? If you could please elucidate. Definitely looking to improve on the next batch.


To answer your question, I didn't ever let the limonene stand for very long on it's own after decanting from the bark mush, but I did filter through a SS funnel with a cotton ball before adding the vinegar, as instructed. If you read carefully through the post I did mention some sort of film or emulsion forming at the barrier between the two liquids. A bit more on that might shed some light here: Not knowing what it was and wanting to investigate, I scooped it carefully out as much as possible with a fine mesh sieve. Outside of the liquid it looked to me like very fine plant matter. Now that you mention it, it did seem to be trapped in a kind of gel. I do believe I got most of it out and it was discarded. The vinegar was likewise filtered through cotton several times after each wash. I do wonder if a coffee filter might not be more consistent /effective.

As for the end product of evaporation- it wasn't liquid, as shown in the pictures on the tek page. I used very low heat, the minimum setting that caused evaporation. What happened is slowly from the ends of the puddle towards the centre the liquid flashed off leaving a waxy film on the glass, even while still hot.

Something else maybe worth noting, after vaporizing some the other night (which definitely was active) I had some residue- a very light tan coloured almost powdery substance, not really a resin. Come to think of it, it's very similar in colour to the gunk I pulled out from between the liquid layers, only now dry. Sound like calcium acetate? It did clean up with water.

I'm using a DT V5 ceramic crucible atomizer on an eLeaf Pico, something I have no prior experience with, and there's a whole learning curve to that as well. I'm going to do a separate post on that but I want to do some more experimentation with it first so as to have something useful to write about. For the time being I don't want to rush and attribute to impurities what could quite possibly be due to poor vaporizing technique. I do suspect I am not getting the material to a high enough temperature, being overly cautious not to burn it. I did some testing today with just the device and a thermal probe that suggest the effective temperature reached is much lower than the (manually calibrated) set temperature on the mod. Makes sense, with the cooling effect of evaporation and cool airflow drawn in by inhalation. Jungle spice directly in the ceramic bowl doesn't seem to work very well. I ordered some ceramic "flavor discs", or a cheaper version of a Healthstone, but I don't have them yet. I'm reluctant to vaporize off of copper or any kind of metal for that matter.
More experimentation is definitely needed.
 
VoyagerGrey
#4 Posted : 9/5/2023 12:38:06 AM
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Quick search on calcium acetate yields the following:

Physical State; Appearance
WHITE-TO-BROWN OR GREY CRYSTALS WITH CHARACTERISTIC ODOUR.

Physical dangers


Chemical dangers
Decomposes above 160°C . This produces acetone vapour and calcium carbonate. Reacts violently with strong acids. This produces acetic acid fumes.

Inhalation risk (powder form)
A nuisance-causing concentration of airborne particles can be reached quickly when dispersed.

So the main hazzard here would appear to be the release of acetone vapour. Not great, but at these quantities/frequency, not that aweful. I've probably inhaled more acetone vapour in an evening sitting next to my GF removing her nail polish...? Probably.

Does make one question the safety of "food safe" extractions though... Just cause you didn't put in anything nasty doesn't mean it's not there at some stage. Kinda like how they add amylase to "unsweetened" drinks or celery culture to "naturally preserved" deli meats.
 
VoyagerGrey
#5 Posted : 9/5/2023 4:41:23 AM
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*Someone* just came back from a rocket ship ride to infinity... or god knows where.

Still some improvements to be made to vaporization technique but Jeezus Christmas that was one of the most intense rides yet taken.

There are some insights to be had into the previous conundrum. Not from hyperspace, but from the kitchen. If downwardsfromzero's guess is correct, lets assume there's some calcium acetate in my tincture, the result of failing to separate excess lime from the limonene before salting.
That would decompose to calcium carbonate and acetone vapour at 160c, so within the same range as spice. Dry, chalky, non volatile residue in the cup after vaporization of everything that will vaporize seems to confirm this. Weighing this should give a ballpark of how much is present in the tincture.

Attempt #1, using 10 drops- or what should have contained 45mg, left somewhere between 17-25 mg of said powdery residue. Quite a bit. The measurement was non conclusive, I think the scale was off balance.

Attempt #2, now aware of the reduced concentration:
After flashing off the vinegar and completely vaporizing 14 drops, The remaining residue weighed in at 28mg.
14X4.5-28=63-28=35
35/63=0.55
0.55*2.52(<-my first estimate based on concentration/volume)=1.386g yield
Some mass would have flashed off as acetone, but my lungs and throat wouldn't know it if no one told them. Still, Myself probably got over 1% yield, so happiness! Steps can be taken on the next batch to avoid this unwanted byproduct, but I'm not too worried, as mentioned in the previous post.

So much for (dubious) math... subjectively, that estimated 32mg-35mg dose, which was not 100% consumed on the first attempt- (there was a bit left to give a nice glowy buzz on vaporization after initial come down). Was just about right. Might try to go higher if I ever get comfortable with this level.

And what-the-even-happened. The only thing I can predictably expect from a ride to hyperspace is that it will be *nothing* like what I expect. Even if I was just there 20 minutes ago. Every time I step through that door, the first (coherent) though my brain can form is
"Oh yeah. Remeber how last time you thought you'd remember what is was like? Well, how about that now?"Big grin
 
 
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