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Ethyl acetate approach Options
 
merkin
#1221 Posted : 5/13/2022 7:03:53 AM

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Thanks for the details there orchidist, much appreciated. I am definitely going to experiment with those as I slowly dry and powderise my harvest.

I kinda cocked up my crystals by running the liquid through a vacuum filter. Didn't think it through, just a habit from before when I was using the 'bomb and stir' method which produced powder! Oh well, lots more powder and plants waiting.

After drying overnight at 30°C (about 5° above daytime temp) the weight of the powder ("delicately light crunchy flakes" now rather than crystals) is ~3.3g. Starting weight of powder was 106g. That puts the yield over 3% citrate, somewhat on the high side. And the evap of the DH2O wash of beaker is still in progress. Not significant tho I suspect.

Before anyone gets too excited (me especially) - I may have made one silly cockup - I let through a short stream of whitish 'sludge' on one of the pulls (pressed plunger too hard and wasn't concentrating) that pretty much jammed up the first coffee filter so I poured the contents into a new filter and carried on. I did allow to settle overnight in fridge and filter second time before adding citric (2.5g). Didn't see any residue in empty beaker after decant but could have missed it so I suspect a contam of lime.

If there is some unwanted calcium hydroxide in here how would I clean the powder to remove it?

- - -

Powder source fyi: own plant, over 15 years old, stored almost exactly 1 year in newspaper. Dried full plant except thorns clipped for handling. Have much more pedro waiting too, from various plants (cloned) but similar age. Pedros have way more mass tho obviously.
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orchidist
#1222 Posted : 5/13/2022 7:15:45 AM

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I've found that the calcium hydroxide doesn't stay in suspension for very long in ethyl acetate, I wouldn't worry too much about it contaminating your product by any appreciable amount as long as any sediment you see is decanted off before salting

With regards to sludge, I like to pour out of the press into a beaker before filtering into a second one. That way you can easily decant or pipette the unwanted stuff out. I also use the intermediate step to weigh the output of each pull and record it.

That said, I've found that when using a drying agent (if even just sodium carbonate), any haziness in the solvent from water in suspension goes right away. You can proceed to the next steps much faster.
 
merkin
#1223 Posted : 5/14/2022 3:10:53 AM

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Thanks orchidist. I would still like to try some method to maybe get rid of calcium carbonate (oops, hydroxide not carbonate!) contamination. The liquid was so dark green that I couldn’t really see anything in it and the yield seems too high really. Would I have to AB this with xylene again or is there a simpler method like a solvent wash or re-x that would dissolve the mesc and leave the hydroxide? And if AB how much xylene per g of mesc citrate? Those teks use close to a litre of xylene which seems a bit like overkill but this is out of my knowledge area.
 
orchidist
#1224 Posted : 5/14/2022 5:17:23 AM

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I didn't take a good look before, but those crystals do look pretty different from what I'm used to seeing.

I hate working with xylene and I'm happy to tell you I've got alternatives for you Big grin

The first is to add it into fresh powder and repeat CIELO as normal, the normal dosage of citric acid should be more than enough to crash all of it out, but just to be safe, I'd recommend to use pH paper to be sure the solvent is acidic before you go ahead with collecting product.

The second comes from when we were trying to rule out phytochemicals as the cause of oiling out, I made a thin paste of my product and lime (5 ish grams of lime and just enough water to make everything flow), and extracted back into EA by stirring, settling and decanting. It does not form an emulsion, so it doesn't take long to settle, and you can stir or shake it vigorously. I used a stir plate and the layers separated immediately. You won't need very much solvent, 200ml divided into 3 or 4 portions is likely more than enough. pH paper will show up slightly alkaline if you're still extracting M from the paste. Use that to make sure you've got it all. Filter if the extract isn't crystal clear (pretty confident it will be though), then add your CA.

Use K2CO3 to dry the extract when using this method. I found there was enough water dissolved in the solvent to cause it to oil out.
 
merkin
#1225 Posted : 5/14/2022 7:55:22 AM

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Excellent, thank you orchidist.

I was totally hoping it wouldn't involve xylene and that whole rigmarole - it's why I had old powder stored for so long until Loveall came up with this tek idea. Previously did about 7g of sanchez the usual old xylene route and didn't really enjoy the process. The result was definitely good, but I kinda drifted more into spice and harmalas after that, forgetting about cacti (although growing them wherever I could plant haha). Loveall awakened it all again and boy am I grateful!

Your first solution just sounds perfectly elegant. And since I am busy drying and powdering three different plants now to finally try them all - they have all been wrapped in newspaper almost exactly a full year - it fits perfectly into the program.

 
Loveall
#1226 Posted : 5/15/2022 9:55:21 AM

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You mean Calcium Hydroxide contamination (not carbonate from a couple posts above)? I agree with orchidist, that it is very unlikely to be in your final product based on the steps you followed.

Dark green can happen and can depend on the plant. Also, darker green can happen if pulling when EA is warm. It should not affect the extraction and you can use a flashlight to help check for debris (if not used already). You can pull with colder EA (from fridge or freezer) to lighten the color of you really want thag (as you may know), but that can lower yields by a small amount.

Congrats on your results. That yield is high but not unheard of. Do you know the specific bridgesii type? Is the 3% yield with core included?

Thanks for the detailed results. Cheers and enjoy πŸ™‚
[center]πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
merkin
#1227 Posted : 5/16/2022 8:35:00 AM

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Thanks Loveall. Yes, Hydroxide. Facepalm. Fixed it. Had to dash off to the 'lab' and check the bottle though to make sure I hadn't been doing something so stupidly wrong!

I am busy with another extraction on the same material so I will compare yield before embarking on the 'cleaning' as suggested, I thought over 3% was excessive but good to know its possible. Increased filtration to two coffee filters per session in case of more emulsion 'sludge'. Didn't notice any this time in the Bridgesii pulls. Same powder from full plant including core.

Unfortunately I have no other info on the Bridgesii plant, I dried and powdered the entire thing incl core (except thorns removed). Since acquiring it I have got four more that were actually named - one called "Ben" from Australia, one "Fourwinds" and the two Monstrose clones - long and short. All are still too young for harvest.

I had a Pedro piece that broke off one of my plants just over a month ago that has been sitting around waiting to get wrapped so I dried it out and am trying that at the same time. I have more that are sitting wrapped from a year ago I haven't got to yet, but since this guy was around I chopped and dried. This one was decored but skin & spikes on.

I had quite some water in base of beakers after 24 hrs in fridge! Decanted and filtered. Water seems to stick to beaker for a while. That recommendation is definitely needed! Not sure whether water came from paste or powder, but there was quite a bit. Wasn't apparent until decanted thru filter. Impossible to see, even with a torch (aka flashlight Smile due to dark green color. Will always do this step in future as part of the tek.

When pulling the Pedro I saw the same 'sludge' (opaque green and denser than clear EA) I got earlier with the Bridgesii. Probably emulsion from pressing plunger too much? I avoided decanting it into the filter until right at the end, and then through a new set of double coffee filters.

Interestingly the two looked really different after citric acid added. In Pedro solvent (done first) I saw absolutely nothing in the darkness except some citric acid pieces tumbling and on the bottom edges (I pestle/mortar crushed it this time to facilitate dissolving) and stirred about 40 seconds because I could still see the acid. Within 5 min there was some fine crystaline precipitation at bottom and the sides had begun to sparkle noticeably. When adding citric to Bridgesii liquid there was an immediate and very visible clouding so I hardly stirred it. It exhibits a cloudy green, even with the torch, whereas the Pedro shows that purple-red color under the torch light. Backlit by the torch its still far to dark to let the beam in! Maybe due to its freshness? Anyway, in less than 10 minutes its up and running to fine crystals.

Some pics attached, hope they're as useful to other non-chem noobs like me.

*** EDIT ***

Less than 2 hours in and both beakers looking like previous session took 30+ hours to reach in terms of crystals...guess I'm doing it better this time! Red-purple colour is gradually appearing slowly downwards on the Bridgesii beaker.

Thought: maybe because the solvent was close to fridge cold at time of adding acid?
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downwardsfromzero
#1228 Posted : 5/16/2022 9:14:54 PM

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Very nice!

Settling time seems to be as crucial here as it is in harmala extractions, albeit for water as well as particulates.

Cold solvent might have fewer convection currents, maybe that helps with crystal formation?




β€œThere 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."
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Loveall
#1229 Posted : 5/18/2022 12:43:35 AM

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Great results merkin πŸ‘

And thank you for sending thanks earlier. Learn, share, expand. A force of creation. That's what it's all about πŸ’—
[center]πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
merkin
#1230 Posted : 5/19/2022 1:02:29 PM

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Loveall, the photos of the crystals you grow seem to be considerably larger than what I am managing - Is there some trick to getting larger ones? My last round I tried not stirring at all (powderising the citric helped a lot) but still the largest clusters seem to be around 6-8mm in width (trying to measure in a beaker with a ruler lol). Just wondering how you do it? When dried in the filter they dry into the needle looking type after coming out in a mushy green blob, similar length of needle though.

For the record, my San Pedro (not kept in dark and only a month since it broke) delivered a yield of 1.87g from 100g powder - dried and powdered everything except central 'core' - so 1.87% which is not as much as the Bridgesii but I'm still quite pleased. That plant I have growing all over the place so it's nice to be able to kinda quantify the garden Smile Will be interesting to see if ones kept in dark for a year yield higher. Probably a good idea to test 'full plant' vs. 'everything but the core' too. Unless of course this has been done to death.

The second Bridgesii extraction (same full plant powder as first run) is drying now. I'll be interested to see if I contaminated it with lime. Judging by the visual results of this one in the beaker I would say I did. Will edit this to add yield when I know.

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Loveall
#1231 Posted : 5/19/2022 3:28:40 PM

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Those xtals look perfect to me Smile

Great work, and yes very interested in any core vs skin data. Aging data too.

Cheers and happy extracting. Remember to wash and reuse the solvent if not doing so already πŸ’š
[center]πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
merkin
#1232 Posted : 5/19/2022 5:07:05 PM

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OK, thanks Loveall. I will definitely try variations on skin+flesh with core or without and the aging. Have plenty material from those two plants to use in both forms.

To update my first Bridgesii extraction it seems I definitely let some of the emulsion 'sludge' get into the final jar. Using a single coffee filter allowed it to come through and in the decant after settling I think I absent mindedly swirled a bit to much while pouring into the filter. I couldn't see much in the liquid it was so dark. When emptying into the buchner funnel at the the end there was a thin crust at the bottom of the beaker which came out in large flaky chunks. Must have been lime that passed through filters. I promise to be more careful! And definitely I am doing it better already and way more careful on the final decant/filter. This is so much more satisfying than the 'dump and stir' method I did last year Smile

Final yield of the second extraction from the same Bridgesii material (full plant, 'aged' 1 year) was 2.276g off 100g powder so 2.276%. Not over 3% but I'm still more than pleased with that, and it's all 100% light fluffy crystalline, zero flakes. The final hot water rinse of the beaker is still evaporating but I don't expect too much from that. Last time was around 50mg.

I have some powder from Bridgesii and Pedro left and will make it up to 50g with new and run the results of the previous 3.3% yield through that extraction as well to compensate my sloppy tek execution.

Definitely I will re-use solvent. It gets consumed fast! I have about 2 litres cleaned so far, and now I'm trying the activated charcoal to clarify. Wish I had a bigger sep funnel!

Should I also dry the used solvent after filtering the charcoal out?
 
Loveall
#1233 Posted : 5/19/2022 7:13:58 PM

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I don't dry the solvent and don't have issues. I stopped using charcoal and just use it dark, has been working fine. Super simple πŸ™‚
[center]πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
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