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Sausages
#1 Posted : 8/30/2020 1:59:28 PM

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So, this is what I did this weekend! This is not an extraction guide or tek - this is just a description of what I did, basically so everyone can tell me what I did wrong, and maybe some people can learn from my mistakes.

For better or worse I felt like trying the whole extraction process for myself without stopping and asking questions at each stage and ending up second-guessing everything. At first glance I thought I'd be performing a scaled-down version of the lextek, but Northerner steered me towards Cyb's tek and also suggested the use of a pressure cooker for the acid cook. It was also suggested that the defat be performed twice. For the most part this follows Cyb's tek; What I'm doing seems more their hybrid tek but I've been reading the max ion tek because it includes the defat step. The preparation of the material differed as I am using more than just root bark.

Materials:
-Source material - A hefty branch, removed from a cultivated, youngish A. longifolia in full bloom, Mid-August after heavy rain. This is reportedly a bad time to be harvesting but it is a good time to identify the species.
-Demineralized water
-NPS - Shellite - Calcium Chloride added to ensure dryness. MSDS reports 70-100% naphtha, 0-30% hexane.
-Acid - White Vinegar - cheap, presumably distilled. Could not locate MSDS for this product.
-Salt - Natural Cooking Salt - presumably non-iodised. Could not locate MSDS for this product.
-Base - Lye - MSDS indicates 98% purity is the maximum obtainable, did not specify what may be in the 2%
-Litmus paper - I haven't used this since high school and can't vouch for the accuracy of the material used.

Preparation of plant material.
The phyllodes and flowers were stripped off and the bark removed from larger stems. Green twigs were cut up. The material was thoroughly dried at ~70 C in a food dehydrator overnight, then ground up and weighed at ~200 g. The material was placed in a blender, demineralized water was added to cover it and the mixture blended. The ~750 ml of mixture was placed in the glass flask from a large drip coffee maker (the flask) and placed on the coffee maker's hot plate for an hour for gentle heat. The mixture was then placed in a plastic airtight container and placed in the freezer overnight. It was thawed and frozen again for a total of 3 freeze/thaw cycles, then kept refrigerated until preparations were complete for the next step. Appearance - resembled green porridge.

Acid Cook
Water and vinegar was added to create 1.5 L of material with a pH of ~3. The material was poured into a 4.5 L stovetop stainless steel pressure cooker and brought up to it's operating setting on a high heat (from user manual - 119°C, operating pressure 95 kPa, regulating pressure 130 kPa) then kept at that setting on a low heat for 40 minutes. The cooker was allowed to cool naturally for an hour then any remaining pressure released and the solution strained from the material with a stainless steel sieve, then again filtered using an extra-strong, extra-thick paper towel. The process was repeated two more times, adding 1 L of acidic water each time. The filtered solution was combined and reduced over a low heat in a stainless steel pot down to ~500 ml of material. Mixture was covered and allowed to cool to a warm temperature, then placed in a 1 L jar. Appearance was similar to rich beef stock.

Defat #1
100 ml of NPS was added to the jar and gently agitated for 30 seconds.

Here's where I hit what I thought was my first snag - the NPS layer. I had noticed some minor foaming occurring after pouring the second acid cook product into the pot but thought little of it at the time. After mixing the solution the NPS layer looked like something of an emulsion. While I think I understand what the extraction process actually does, I still feel like I'm cargo culting things a little at this point, and so I tried two things that had been mentioned with regards to emulsions - salt, and vibration. Some salt was added and the solution rolled around in the jar, which didn't seem to make a difference. The vibrating device used (in this instance, a head massager) seemed to push the emulsion around and leave a clear patch of NPS. The emulsion seemed to be confined to a clearly defined NPS layer rather than the whole thing, so I proceeded with separation. Then I hit my second snag - my turkey baster was not very effective for removing the top layer. So instead the bottom polar layer was siphoned out from underneath using 2 m of plastic tubing and another identical jar to collect. and the last part separated using a baggie with a pinhole in the corner as a separatory funnel. A small slick remained on the surface of the solution - this was mopped out with a paper tissue. No further NPS seemed to be present. It dawned on me that the "emulsion" I was looking at what could be the fats I was trying to get out.

Salt
90 g of salt was added to 300 ml of near boiling demineralized water, and 200 ml of the salt solution was added to the jar. At this point I got confused between Cyb's Hybrid ATB tek and their Max Ion tek. The latter calls for a litre of salt water but I don't have a glass vessel that will hold the total amount; my largest vessel is the coffee flask (which I don't want to use for pulls), followed by a pickle jar that will hold approximately 1 litre.

Basify
Gloves and glasses on for this part and pretty much everything past here! 50 g of Lye was added to 200 ml of cold demineralized water, dissolving 10 g at a time. The solution was transferred from the jar to the coffee flask. The lye solution was added to the flask and the mixture stirred. pH was tested and appears to be ~14. The solution darkened on adding the lye and a soapy aroma was noticeable. Cyb's tek mentions adding more demineralized water but I used a bit too much salt solution and my jar would not hold everything; I'm guessing it won't be a problem. The flask was placed on the coffee maker's hot plate for 2 hours, stirring occasionally. A very small, slightly frothy, reddish slick appeared on the top of the solution. The flask of solution was then left to cool overnight.

In the morning I bought a few more things - a bigger jar (1.5 L), a more precise measuring jug from a hardware store (plastic but unlike ones sold for kitchen use, was labelled as safe for use with chemicals including solvents), and a syringe (I was hoping to get a glass dropper, but the local pharmacy was out of stock).

First Pull
The solution was transferred to the 1.5 L jar. ~50 ml of room temperature NPS was added and the jar lightly shaken then rolled for 30 seconds, this was repeated 6 times for a total of 300 ml of NPS. The jar was placed in a heat bath (a small cooler full of warm water). Most of the the basic solution was siphoned out from underneath and the remainder of the material placed into a smaller jar. A baster was used to remove most of the NPS layer, the syringe was as the level dropped, and a bag was used as a separatory funnel for the very last part. The basic solution was kept in a jar, labelled, and safely stored. I then realized that this part was overly rushed and I wasn't paying attention to the tek, but as pulling was going to be repeated regardless, I continued with my extraction. The NPS was placed in a different jar and refrigerated.

At this stage the original plan was to re-acidify, perform another defat, then re-base and do a final pull. However the NPS at this stage seemed to have a distinct odour beyond that of the NPS itself, so it was decided to see what ensued if precipitation was attempted at this stage.

Freeze Precipitation
2 Pyrex pie dishes were pre-cooled in the freezer overnight. Approx. 50 ml of NPS was placed in each pie dish, covered with clingwrap, The NPS remained clear as it was added to the dish. The jar with the rest of the NPS and the dishes were placed in the freezer and left undisturbed overnight, around 18 hours. I suspect my freezer is very bad for this sort of task, the automatic defrost system seems to spread the solvent fumes pretty badly, I will be investing in some pyrex dishes with covers for any subsequent work. The dishes and jar were removed from the freezer, the NPS was cloudy but no crystals were apparent. The utensils were drained, and put in front of a fan to dry for a half hour. Only the slightest of films appeared to be present on the dishes and jar, not even enough to scrape properly. Expectations were very low but it would have been nice to see anything come out at this stage. The remainder of the NPS was evaporated in front of a fan in open air, some water appeared to be present and was also evaporated. Scraping produced a tiny amount of yellowish gunk, an uncalibrated 0.01 g scale showed 0.04 g of product.

Preliminary results
Product was smeared onto some stainless steel scourer that had been burned clean and placed in the machine with the gunk towards the inside. Heat was applied and a vapor given off that tasted plasticy but tolerable enough, and the vapour was inhaled and held in for ~30 seconds. No noticeable effect.

Second Pull
The solution was transferred to the 1.5 L jar. 100 ml of NPS was added and the solution agitated and rolled, then left alone for a half hour or so in a warm bath, and the process repeated about 8 times without adding more solvent. The NPS settled into a yellowish layer, the majority of the base material was siphoned out, and the remaining 100 ml solvent and approx 100 ml base layer were moved to a smaller jar. The solvent was removed with the baster, then with the syringe, then with a baggie funnel. The solvent was placed in a pyrex dish and left in front of a fan for several hours. The thin layer of goo was weighed at 0.06 g on the uncalibrated scales, with a tiny amount still present on the dish.

Testing
The stainless steel mesh from the machine was used to try and mop up the small amount still in the dish with limited success. The goo from the scraper was smeared onto the mesh and a little more material was scraped off the dish but not weighed, and again put onto the mesh. Heat was applied using a lighter and the vapor inhaled and held in for about 30 seconds. No discernible effect.

What I think I've learned
I'm extremely disappointed in myself for the lapses in safety.
I'm happy with how I prepped the plant material but now think I should have gone for the long slow cook instead of using the pressure cooker.
It's very important not to get distracted while performing any work. I was extremely lucky not to injure myself despite thinking I was being mindful of safety.
Patience is a virtue, unfortunately it's not usually one of mine, but waiting seems like a form of excitement during the process.
I may need a better freezer.
Proper lab glassware, particularly a separatory funnel, would be awesome but I'm unsure how to go about procuring it without drawing unnecessary attention. I do have a couple of friends who do legit chemistry work I can ask about that, but at present it's not in the budget anyway.
Round dishes are more frustrating to scrape the edges of than I expected.
Extractions are fun to do.

Looking Forward
The plan now is to do a few more pulls, defat again as was recommended to me, and hopefully get some actual crystals to experiment with. I will try freeze precipitations again once I have a covered dish, but I suspect my freezer is not capable of dropping the temperature low enough. Despite the lack of success I'm happy to have gotten the practice and more familiarity with the process. Aside from that I'll be waiting until summer before collecting any more plant material to experiment with, as well as trying different source. DMT-containing Acacias don't seem to be either native to my local area nor common, but I think I've identified this one accurately as well as some A. floribunda; possibly an A. maidenii as well but that may merely be a misidentified floribunda. Or something else, I could be way off. Assistance with ID would be appreciated.

Safety Notes
There was some mucking around and lessons learned about siphoning - it is very important not to siphon caustic materials using your mouth! I forgot this part from my education. I got distracted while siphoning and got to taste a small amount of naphtha/acid emulsion, bleh. But if this had happened with a stronger acid or with a basified solution the results could have been dire. I've amended the health and safety wiki page to include a note about siphoning. A few drops did end up splashing onto the gloves as well as inadvertently resting part of my hand on the base-covered rim of a jar, proving the importance of PPE.
A stable workbench is essential. I preferred to do some of the procedures in my garage rather than the house due to odours; however the folding table I had as a bench was not sufficiently stable for performing this sort of work safely, so work either had to be done on the ground instead, or brought back into the kitchen.

Other Notes
I feel a little embarrassed about sharing this failure but OTOH somebody might find this useful and the nexus seems to consistently give appropriate and informative feedback. Apologies for not taking photos but I felt that documenting this photographically would be both a distraction and a privacy risk. In future I will find ways to mitigate the latter. As this is my first extraction I thought I'd more or less stick to what's been recommended; I deviated from Cyb's teks in a couple of places but aimed to more or less follow their example. Apart from a DXM extraction many years ago I haven't done any chemistry work since high school.


Questions
Any further advice regarding the use of acacia phyllodes and other non-rootbark material would be highly appreciated. The specimens near me are not numerous, and they are also in highly public areas (not the botanic garden specimens from my acacia thread post, I consider those specimens to be off-limits), so I am not interested in trying to get their rootbark, but I am happy to discreetly help myself to a branch or two.

Gratitude
Thanks for reading! Also thanks to Northerner for their advice in my intro thread; Cyb for their teks including their machine design which inspired my own one; whoever is responsible for the Lextek, that wasn't used but it was still quite informative; The South Aussie Shroomery folks for their encouragement, The admins for keeping this site going, the countless people whose posts have inspired, educated and entertained me, and my lovely partner for putting up with me through all this.
The stars keep burning,
Worlds keep turning,
Through joy and pain,
Forever learning.
 

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Psyzsee
#2 Posted : 9/8/2020 6:11:12 AM

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Did you do the like the Pedro thing like sub zero mortal Kombat it first and then like do everything I think?
 
Sausages
#3 Posted : 9/11/2020 12:46:09 PM

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I'm not sure what you're actually asking.

I've attempted another extraction, this time from Acacia floribunda bark and branch tips exclusively, from branches of various sizes that had no phyllodes. I experimented by doing 3 batches - 1 was 100g of bark, with a defat after the acid cook. 2 was 50g of bark, doing a mini A/B instead of defatting. Both of these were cooked for a long time (12+ hrs) at a low temperature (below boiling), then the combined bark was moved to a pressure cooker for another acid boil at high temperature for batch #3. I also experimented with using sunflower oil as the NPS on batch 2 as well for the last attempted pull.

Despite the naphtha becoming cloudy this time, the end results were dismal, with minimal amounts of inactive goo from batch 1, a mere smidgen of inactive goo from batch 2, and I haven't tried pulling anything from batch 3 yet. I seemed to get ice crystals in the dishes during freeze precipitation, despite having lids for the dishes I was using, and my freezer doesn't seem to go lower than 15°C so after leaving things in there for a week and seeing crystals, tried evaporating with the results mentioned above.

I worried that filtering out the solids has had an adverse affect but that doesn't seem to be a problem looking at various teks. It could be that the source material has no active tryptamines, but I do have one local person who vouches for the A. floribunda in the area. It's also possible that the shellite is failing as a non-polar solvent. Though the MSDS indicates it should do the job (being a naphtha/hexane blend), on the forums it sounds like shellite is not the product it used to be. There seems to be only one brand available that I've seen at hardware stores, though another brand whose MSDS indicates commercially pure naphtha is apparently available from industrial suppliers, they're not in my area. I'm not sure whether to try xylene which sounds like it requires a full evap, or try a lighter fluid and hope it's naphtha. I'm not sure if I have access to other NP solvents other than vegetable oils, which don't allow freeze precipitation or evaporation.

I'd appreciate any input from people who have had such a problem and found a solution to it. At this stage I'm not likely to try another extraction until summer.

The stars keep burning,
Worlds keep turning,
Through joy and pain,
Forever learning.
 
potnoble
#4 Posted : 9/11/2020 1:30:01 PM

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Hi Sausages

I am no expert but if you get ice crystals in your pyrex either your solvent has some water in it
or you haven´t sealed it air tight.
A regular freezer should be enough for this.
Maybe this specific bark has very low levels of desired alkaloids.

The solvent i always used has changed and is now impossible to work with.
So you should probably check on that, too.

Anyways i wish you good luck with your next try.

Have a gud one
I smoke cheese
that makes me look japanese
 
Sausages
#5 Posted : 9/17/2020 5:50:08 AM

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Thanks potnoble, I think poor sealing was the issue with the ice.

I've tried another pull with xylene, which produced a small amount (<0.1g) of yellow goo that was loaded into the machine and smoked with no noticeable effect. It's quite possible that the source material was no good, I will try again in the summer when the alkaloid content is supposedly at it's peak. That will also give me time to acquire other NP solvents to trial.

I'd much rather keep trying my own harvesting and extractions rather than source DMT or even rootbark from an appropriate supplier.
The stars keep burning,
Worlds keep turning,
Through joy and pain,
Forever learning.
 
 
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