Touche Guevara
Rising Star
So how would SWIY compare this to the traditional STB? Does using CaOH instead of NaOH make things more difficult, or does the limonene/drytek aspect make up for the less corrosive basifying agent?
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Nontoxic Extraction Experimentation Log w/ Photos (tek WIP)
- Thread starter amor_fati
- Start date
SWIM couldn't say for sure at this point, but he believes the strength of his technique to lie in how completely the blender pulverizes and blends the material. The base doesn't necessarily have to do much work on the material itself apart from providing a thoroughly base environment throughout; however, SWIM's always understood lime to be a potentially harsh base on plant material. Another advantage would be that there's less volume to have to disperse the limonene in, so less limonene can be used for adequate results. Of course, it's still early in experimentation to claim any of these for certain, but there's very little doubt in SWIM's mind regarding this.
SWIM went ahead and authored a tek. He'll remove the warning after he gets all of his results posted and add some photos and convert it to a pdf, but he will continue work on it and release subsequent editions, as developments arise and culminate.
SWIM went ahead and authored a tek. He'll remove the warning after he gets all of his results posted and add some photos and convert it to a pdf, but he will continue work on it and release subsequent editions, as developments arise and culminate.
mumbles said:
The most I could find regarding this is that with some metals, there is the possibility of a reaction that produces hydrogen gas, but most MSDS's don't even list this as a hazard. SWIM hasn't noticed any corrosion to the blade assembly whatsoever, nor does he think that any amount of metals would dissolve in limonene. Any reactivity between the blade assembly and lime is likely either negligible or nonexistent. SWIM would imagine that this may be a bigger problem with more exotic metals.
A few brief notes on the process:
-for the collection jar, it's best to put the lid's rim on loosely and insert the neck of THP through that, as this will prevent a seal from forming between the bottle and the jar and slowing down filtration.
-SWIM had a bit too much material in THP, making it difficult to stir without losing limonene from overflow, though he suggests using only 100g MHRB, if too much is used (definitely try to use no more than 150g), excess can simply be removed and placed in the blending jar. Since this jar will be used in transferring limonene for every wash, the excess can be stirred in with the limonene, prior to decanting back into THP, to ensure a thorough extraction.
SWIM's thinking that for this process, in order to save on limonene, if a bulk amount is being extracted, that one determine the total amount of limonene to be used in total beforehand. That amount can simply be prepared in a jug or bottle and distributed between each separate extraction as need be, and if the extract same process, consistency and amounts are used in each one, there would be no need to gauge each one individually; thus, the total amount of limonene can be collected and salted all at once. SWIM sincerely feels that if only a day were dedicated to the extraction process, this could yield incredibly decent overnight results.
SWIM has one other idea that may work for this, but he won't be able to test 'til next time: The use of a small electric mixer (like one used for mixing/kneading dough) could greatly speed up the stirring and filtering in THP, especially for running several extractions at a time.
SWIM will have the final verdict on the first trial quite soon, then he will use the same limonene on the second (which will be essentially identical). He may use the same for the third, simply to conserve, but he'll reserve that decision for when the time comes.
Edit:
SWIM wonders if by fitting a nozzle to a rubber band and rapping it to seal the loosened lid rim to the collection jar, one could connect an air pump to generate negative pressure.
-for the collection jar, it's best to put the lid's rim on loosely and insert the neck of THP through that, as this will prevent a seal from forming between the bottle and the jar and slowing down filtration.
-SWIM had a bit too much material in THP, making it difficult to stir without losing limonene from overflow, though he suggests using only 100g MHRB, if too much is used (definitely try to use no more than 150g), excess can simply be removed and placed in the blending jar. Since this jar will be used in transferring limonene for every wash, the excess can be stirred in with the limonene, prior to decanting back into THP, to ensure a thorough extraction.
SWIM's thinking that for this process, in order to save on limonene, if a bulk amount is being extracted, that one determine the total amount of limonene to be used in total beforehand. That amount can simply be prepared in a jug or bottle and distributed between each separate extraction as need be, and if the extract same process, consistency and amounts are used in each one, there would be no need to gauge each one individually; thus, the total amount of limonene can be collected and salted all at once. SWIM sincerely feels that if only a day were dedicated to the extraction process, this could yield incredibly decent overnight results.
SWIM has one other idea that may work for this, but he won't be able to test 'til next time: The use of a small electric mixer (like one used for mixing/kneading dough) could greatly speed up the stirring and filtering in THP, especially for running several extractions at a time.
SWIM will have the final verdict on the first trial quite soon, then he will use the same limonene on the second (which will be essentially identical). He may use the same for the third, simply to conserve, but he'll reserve that decision for when the time comes.
Edit:
SWIM wonders if by fitting a nozzle to a rubber band and rapping it to seal the loosened lid rim to the collection jar, one could connect an air pump to generate negative pressure.
Well here's the results of the first non-toxic trial: SWIM retrieved 1.8g with 1g or less of fumaric acid, so 0.8-1.0g freebase, bringing the total to around 2g, meaning about 1.25% yield. Keep in mind that SWIM hasn't purified this yet, but he crystallized it the same way he did the previous purified yield; it's nearly the same consistency, so SWIM would guess that no more than .5g fumaric acid would be removed by purification (so, about the exact yield as from the previous pull). SWIM may wait 'til he has his entire yield from the non-toxic trials to do a purification; he'll do it slowly and purify the lye yields alongside the non-toxic for a final comparison.
In terms of % yield, this first trial's neck-and-neck with the lye trial. The major differences in the processes that SWIM's been noticing are how much easier it is to not have to separate limonene from lye water, using much less limonene, and not having to deal with huge quantities of (toxic) liquid. The advantage of the lye process however, is that SWIM can just leave it in the jug and shake it every now and then throughout the week prior to salting.
If SWIM had a whole day available to him to work on nothing but his non-toxic extractions, he's certain that he'd be able to knock out both of the other trials overnight. Next time, he'll be sure to try this: Going from whole MHRB to purified fumarate in a day. In any case, this seems to work just as well as lye, but with a few advantages.
SWIM would love it if someone could try a repeat of this experiment while he's finishing up the other two trials, so he can get some second opinions and some verification of the tek's reliability.
In terms of % yield, this first trial's neck-and-neck with the lye trial. The major differences in the processes that SWIM's been noticing are how much easier it is to not have to separate limonene from lye water, using much less limonene, and not having to deal with huge quantities of (toxic) liquid. The advantage of the lye process however, is that SWIM can just leave it in the jug and shake it every now and then throughout the week prior to salting.
If SWIM had a whole day available to him to work on nothing but his non-toxic extractions, he's certain that he'd be able to knock out both of the other trials overnight. Next time, he'll be sure to try this: Going from whole MHRB to purified fumarate in a day. In any case, this seems to work just as well as lye, but with a few advantages.
SWIM would love it if someone could try a repeat of this experiment while he's finishing up the other two trials, so he can get some second opinions and some verification of the tek's reliability.
Attachments
mumbles
Rising Star
Really looks like it needs to be recrystalised. From the look of the pyrex dish swiy is alloying too much solvent to stay on the plate and crystals, leaving those telltale sticky oily ridges. Use a small glass bowl and pour off as much of the solvent as swiy can after the 48hrs then put it back in the freezer upside down and tilted to one side, leave for an hour or two, take out and remember which point of the dish was tilted downwards and while keeping that shape place it in front of a fan to warm up and dry the condensation, then finally turn upright and allow to dry. This way the oily gunk from your photos will only be around the rim of the glass dish and you will have much much cleaner spice. Swim's pet hate when it comes to this forum is people quoting yields of dirty products.
mumbles said:
SWIM's well aware of how to purify fumarate, and the first 1.4g was purified, but crystallized with haste. SWIM knows approximately how much fumaric acid is in each (whether bound to the DMT or not), but only approximately due to over-saturation of the prepared FASW; he always seems to overestimate the amount of acid when it comes to the results after purification. The color of the crystal does not necessarily denote purity, just a lack of uniformity in the crystal structure from the haste of crystallization. These crystals are solid rocks, not a whole lot different in appearance from acetone washed fumarate, but more solid.
To make these, SWIM evaporated completely in a food dehydrator, then to avoid shooting sticky shards outside of the bowl, he added a little bit of water, scraped it into a pile and put it back in the dehydrator. With the first one, SWIM dissolved the fumarate in water, decanted off of the fumaric acid, and crystallized in the same way. How are these in any way dirty, apart a slight excess of fumaric acid in the second? What could have possibly transferred between the limonene wash (completely devoid of a polar layer) and the FASW that would make it so dirty or throw off the weight of the yield in any way?
SWIM's offering this information to track his progress in the experimentation, not to win a crystal-growing contest. When he's finished with this experimentation, he will purify both the lye and non-toxic yields in the same way and grow the crystals slowly. Perhaps that will indicate some impurities, but SWIM doubts it.
mumbles said:
No problem, it's just that SWIM's been working with the fumarate for quite some time (since the early days of FASA), and so he's become quite familiar with it. In the end, it is possible that there's some kind of impurities that haven't yet been encountered, but it's highly unlikely.
SWIM would imagine the ridges to be fumarate dried thin, but likely with the bulk of fumaric acid contamination as well. Those ridges are quite thin.
SWIM's last pull was done using a combination of the first and second nontoxic trials (vinegar/heat treated). The amount of MHRB being used from those is anywhere between 280-320g total, but SWIM assume a round 300g. SWIM pull yielded almost 3g of impure product, so assuming 1.5g of fumaric acid would mean 1.5g freebase product. Added to previous pulls of the first trial's 2g, 3.5g would indicate the holding steadily over 1.1% (previously 1.25% from the first trial alone).
SWIM would like to point out that he's been delayed with this experimentation due to school and other projects, and that the bulk of the work he's done with these extractions has been over a constrained two-day period. SWIM's getting incredibly decent yields with a very minimal of time and effort.
SWIM's considering purifying the total yield from the the first two trials alongside what he's gotten from the lye extraction just to confirm his current numbers, continuing with all three nontoxic trials, and combining them for the sake of expediency. The amount of material in the lime STB (limtek) trial#3 should be a bit more than the first two, so if the total yield turns out much less than expected, it's likely due to an incomplete reaction on that trial. If it turns out as expected, SWIM's next experiment will have measured amounts of material and reagents, and he will likely do half a kilo all in that manner with no vinegar.
SWIM's been delayed with the final results from the lye extraction, as his attempt at FASIPA didn't turn out. He ended up with a very thin layer of goo on the bottom and no crystal formation at all. SWIM did neglect to cover the jars this was performed in, but there really wasn't much of a layer on the bottom, regardless. He used water to recover everything from the jars and the limonene, and it did turn milky upon first contact with the jars; SWIM'll just evaporate the water to recover the fumarate.
SWIM would like to point out that he's been delayed with this experimentation due to school and other projects, and that the bulk of the work he's done with these extractions has been over a constrained two-day period. SWIM's getting incredibly decent yields with a very minimal of time and effort.
SWIM's considering purifying the total yield from the the first two trials alongside what he's gotten from the lye extraction just to confirm his current numbers, continuing with all three nontoxic trials, and combining them for the sake of expediency. The amount of material in the lime STB (limtek) trial#3 should be a bit more than the first two, so if the total yield turns out much less than expected, it's likely due to an incomplete reaction on that trial. If it turns out as expected, SWIM's next experiment will have measured amounts of material and reagents, and he will likely do half a kilo all in that manner with no vinegar.
SWIM's been delayed with the final results from the lye extraction, as his attempt at FASIPA didn't turn out. He ended up with a very thin layer of goo on the bottom and no crystal formation at all. SWIM did neglect to cover the jars this was performed in, but there really wasn't much of a layer on the bottom, regardless. He used water to recover everything from the jars and the limonene, and it did turn milky upon first contact with the jars; SWIM'll just evaporate the water to recover the fumarate.
Attachments
SWIM's recovered FASIPA attempt yielded 3.7g of material. SWIM's going ahead with purification of both the lye yields (what's left of them:lol: ) and the nontoxic, though neither are completely finished yet. SWIM just wants to confirm his current numbers and quality of yields. Also, the lye extracted stuff's probably not going to last much too much longer, as SWIM and his buddies are utter fiends...so while he still has a hefty amount, he'd like to do some comparisons.
SWIM neglected to record freebase weights, but looking back, he appears to have had around 3.3g freebased from the total lye yields. So that on top of the calculated freebase content of purified yields will give his current % yield from the lye (likely 1.5% or more). With the nontoxic, he should be above 1.1% (from only 3 pulls on the first trial, and 1 on the second), but this purification will give a more precise number. He won't have the final results 'til after the third trial (which will actually be his fourth pull on the first, second pull on the second, and first on the third, so he's expecting quite a haul), however. SWIM's hoping to have all the results in a week's time, and then he'll open a thread for the tek.
SWIM neglected to record freebase weights, but looking back, he appears to have had around 3.3g freebased from the total lye yields. So that on top of the calculated freebase content of purified yields will give his current % yield from the lye (likely 1.5% or more). With the nontoxic, he should be above 1.1% (from only 3 pulls on the first trial, and 1 on the second), but this purification will give a more precise number. He won't have the final results 'til after the third trial (which will actually be his fourth pull on the first, second pull on the second, and first on the third, so he's expecting quite a haul), however. SWIM's hoping to have all the results in a week's time, and then he'll open a thread for the tek.
biopsylo said:
Yeah, but SWIM gets a little too comfortable with it and tends to improvise a bit more than he should. It's all just too much fun! Hopefully now that he's closing in on exactly the sort of tek he's been dreaming of, he can focus more documentation rather than innovation for the next one.
Normally, he probably would have forgone the whole lye thing all together, but he hadn't had a decent amount of spice in some time and was still a little leery of his original plans for experimentation. He wanted a sure thing and hadn't foreseen the development of such a reliable tek, but it turned out as a good opportunity to get a side-by-side comparison, in ease of process and success in results. SWIM's already ready to put away lye for good (he doesn't like the large volumes of liquids, the hazards of lye, the strain of separating solvent from soupy lye water, or the prospect of disposal), and he hasn't even necessarily completed that extraction.
He's thinking of reverting the tek to more accurately reflect the process he happened to utilize (though would have done it differently, had he known), while keeping the more ideal version of the tek that he's currently presenting on the table for later confirmation.
The results after purification so far are: 4.922g DMT fumarate from nontoxic trials 1 and 2, meaning about 3.7g freebase from aprx. 300g MHRB, so 1.25% yield. 5.446g fumarate from the lye extraction, meaning 4.14g freebase plus about 3.3g freebased, so 7.44g total freebase from 500g MHRB, meaning 1.488% yield. Looking very good so far, and the product obtained from each is almost indistinguishable. SWIM did perform a hasty evap/rextal again, so no pretty crystals, but certainly a fairly pure product.
SWIM feels that he can get more than double this load by the time he does his next pull from the next trial, which would put him over the current lye yield. He'll see about getting a bit more out of the lye extraction; he's seriously growing quite weary of it, but he'll do it, anyway, for science!
SWIM's also nearly ready to pull from his salvage attempt from the botched chaliponga extraction from the beginning of the thread using his current methods. Once he's completed that and everything, he'll collect all his used limonene from these along with his pipe cleanings and attempt his first zinc redox in an acetic acid solution; then he'll basify with sodium carbonate, pull with the same limonene, and attempt another FASIPA. If all that works out, it should be a fairly wild product, considering the combination of chaliponga and jurema.
SWIM feels that he can get more than double this load by the time he does his next pull from the next trial, which would put him over the current lye yield. He'll see about getting a bit more out of the lye extraction; he's seriously growing quite weary of it, but he'll do it, anyway, for science!
SWIM's also nearly ready to pull from his salvage attempt from the botched chaliponga extraction from the beginning of the thread using his current methods. Once he's completed that and everything, he'll collect all his used limonene from these along with his pipe cleanings and attempt his first zinc redox in an acetic acid solution; then he'll basify with sodium carbonate, pull with the same limonene, and attempt another FASIPA. If all that works out, it should be a fairly wild product, considering the combination of chaliponga and jurema.
Attachments
SWIM's final lye pull yielded 1.7g more, so 1.7% yield. SWIM's purifying his first pull from the third trial (along with continued pulls from 1 & 3), but it already looks like about 3g, which set the nontoxic trials back above 1.2%; another few grams will catch it up with the lye extraction.
SWIM's not quite finished with the extraction, but he decided that 1.2% from 500g is sufficient yield to officially release the tek: amor_fati's Nontoxic Approach to the Extraction of DMT - Eco friendly extraction teks - Welcome to the DMT-Nexus
SWIM got 1.47g more of fumarate, and re-weighing the entirety of the nontoxic yields gave 9.092g, meaning 6.91g freebase. So the final yield is aprx. 1.38%, which is about .3% shy of the lye pull; but SWIM couldn't say for sure what the weight of the material used for each was (aprx. 500g each), so it's best to say that their well within range of each other. This tek has proven to be a viable nontoxic alternative. SWIM will likely perform one more experiment before the end of the Winter, and the results of his chaliponga salvage are on the way.
Here's a photo of SWIM's final nontoxic yield. He will probably perform a slow recrystallization of this prior to using it for pharma to ensure an even alkaloid profile.
Here's a photo of SWIM's final nontoxic yield. He will probably perform a slow recrystallization of this prior to using it for pharma to ensure an even alkaloid profile.
