oil oil oil man.
Extreme's Excessive Water Spice Extraction
Posted 16 April 2009 - 05:57 PM
I've also been curious about the solubility of the oils in acetone.
I know that freebase DMT is soluble in acetone
Perhaps the oils are not soluble.
If this is the case, one could just dissolve their oily spice in the acetone
Then pour the acetone off the insoluble oils
I think my friend has some oily stuff lying around somewhere
Maybe I can convince him to give it a try.
Posted 16 April 2009 - 08:32 PM
During the process the defat was avoided. he didnt want to risk any chances for big problems too early in the game with working with so much potential end product but if tried again which he personally will not a defat or something additional must be done.
Posted 16 April 2009 - 11:43 PM
thats very strange, i have run total grunge through the heptane recrystalization and got perfect shards out with one go. Naphtha on the other hand never did me any good for recrystalizing, nothing ever came out much cleaner than before.
defats are essential in my opinion, they are so quick, so easy, and by far the best shot you will get at removing those pesky oils, rather than fuckin around with em later.
your choices in acid may have contributed to your excessive oil, i used to use vinegar, then i was urged to go with ascorbic, i wont be going back, vinegar ripps all kinds of oils and tars and odd shades of black out of mimosa that ascorbic simply does not pull out, ascorbic yields just the same in my experience.
Posted 17 April 2009 - 12:13 AM
but wow those white crystals blow my MIND!! so BEAUTIFUL!!!!! wow!
Posted 17 April 2009 - 07:59 AM
Btw, my friend, and many others, have found the solubility of dmt in naphtha to be almost 1g per 100ml. so for 250ml 2.2 is pretty much there.
Posted 17 April 2009 - 08:15 AM
Posted 22 April 2009 - 08:12 AM
Posted 24 April 2009 - 01:26 AM
Ok,5 grams was dissolved into 150 ml of bestine. at 135 F everything was completely dissolved. upon recomendation a cooler was prepared at 155 F as a hot water bath. the jar was placed into the cooler and allowed to cool slowly over a few days.
after 2 days the cooler had only reached a temp of 105 F. a clear seperation between impurities and bestine was expected to be seen but was not. what was seen was 1.8 grams of slighly brown(not yellow) but completely translucent crystals. the bestine was poured of and these crystals seperated.
after just a few moments of cooling about 200 mg of basically oils fells out of the bestine. the bestine was again poured off into a new jar which was allowed to cool and sit at room temp all night. about 1.5 grams of yellow opaque crystals were removed. some oil was again at the bottom.
the bestine was poured off into a new jar and placed into the fridge and then into the freezer. after a day about 400 mg of whitish spice was removed. agoin with oils at the end.
now with only about 3.7 grams of the 5 grams accounted for this dude reallhy began to wonder what was up. and why were oils still falling out after being left sit at room temp. if youve seen andy's recrystal the oils clearly fall out before it reches room temp.
He evaped the rest of the bestine and was left with a small puddle of oils that wouldnt show up on a scale. where did the 1.3 grams go. My guess is it was vaporized when it was in the cooler. I know i never do anything with freebase spice over 140 F but he heard that a cooler can be prepared warmer. well it cant. folks, one of the most important recomendations this tek has discovered is this...do not heat freebase spice past 140F
Extreme's very important tip - DO NOT HEAT FREEBASE SPICE ABOVE 140 F
I'm sure it vaporized...positive. But you say Extreme your still left with 3.7 grams of perfectly good spice...wrong!
Wana hear the trip reports...arite using my spice infused mullein leaf tek he prepared 500 mg of the yellow opaque crystals! they appeared to come out beautiful so after the dead show me and a buddy were dead set on taking off I went first here's the report...
I took one hit off the pipe and did not feel much, the taste was really bad tho. So i took another hit and realized this stuff wasnt working right. It tasted like burnt spice...gross old spice and i was not having ANY CEV after the 2nd hit. I felt weird and it did not feel right. i opened my eyes bc sum ppl were like o you started wo us. The stuff wasnt working, it was weird...really weird! I did not want to hit it again! I tried to get closed eye visuals...i saw some slight stuff i saw i shadow lady silhouette in front of me. at that point i was disgusted with the pipe and tapped it out on my hand. the lady in my visuals turned her back on me and was really pissed. i felt so bad and kept apologizing feeling she was mad!
I was reluctant to load my buddy up a pipeful but he really wanted to just like me and well its cool between me and him to try stuff out so just to make sure.
I gave him the pipe and said good luck, i began to pack up the car so i did not see him smoke it. About 2 minutes later he jumped up with a crash with the most freaked out look on his face. I said it got u good huh...he's like dude. something is wrong with thats stuff...it wont stop. im like man you just hit it its gona last a bit. hes like that stuffs bad, its bad. I kept asking what he saw and he just said he saw a checkerboard with the most evil twisted shit goin on...death etc.
At that point i was like ya fuck that stuff...i said im throwing that batch away. upon my recomendation the dude also threw the rest of that 3.7 g's away fast as fuck. I mean the shit was fucked up...really twisted evil bad feeling stuff. I dont know what happened to it but it was just burnt.
So the story of recrystalization ends...5 grams wasted but hopefully some other's will take my recomendations about the heat...keep freebase below 140 F at all times. never go over...you do not want to waste as much or go thru what i did.
Posted 24 April 2009 - 01:59 AM
Exteme's important tip - use pyrex glass!
Ok, so a batch of this was taken to a festival and ten doses were given out for free. 8 to people who have never tried it and 2 to those who had. i repeated they were givin for free with the intent of enlightenment.
Ok, so this first dude who tried it was a firstimer and after givin all the instructions began to take his first hit sitting in a camping chair. the first hit was cool and but the second hit upon exhaling dropped his ass. i mean his head dropped so hard onto his arm sitting on the armrest and he was out...i mean out! half of the group was experienced and the other half was this kids friends who had never heard of it. they had seriously worried looks on their faces but the other experienced half kept assuring him this was normal. however, even tho i was sure it was cool i had never seen anyone drop like that off anything! i mean i was checking just to make sure he was breathing...i wasnt sure. After 5 minutes his friend began to get worried and so was i so i began to shake his shoulder...it took about 10 second to respond, i was a lil freaked, then he responds."HOLY FUCK...WOW!" i mean he got nailed...he loved every second of it. he said he saw the creation of the universe from the beginning.
Upon coming down he turned and looked into my eyes shook my hand and said, "Thank You!" Exactly the same as the other 9 who had tried it that weekend did.
Arite, so me i was really bummed about the hit of that horrible recrystalized spice from the previous post and really just wanted to go to that place. I also felt really bad. this extraction had so far wasted 5.5 g's of spice. The point of the extraction was to do every possible bit of work to conserve as much spice as possible. to be efficient and not wasteful to god's most precious molecule. Before hand i kept apologizing for what had happened...i felt reassurance tho that everything had been done with the correct intent and if i can come on here to help others save thir spice then my work would be justified. I mean that is what this thread is really about...conserving the most of this beautiful resource.
Also, ive had my share of spice experiences, its been months since my last one, and honestly im not sure of how much i get from keep returnong. but i realized i want to visit that place and visit those people like friend visit friends. so i was prepared, i had good intentions.
I took the first hit and held it in. i felt it about halfway thru holding it in...it wasnt as hard on the body as sometimes. the second hit prodused definite CEV and i was hesitant to take the third but know how much more you get. the third hit blasted me to exactly where i wanted to go...of all the dmtverses i was taken to almost the exact one i wanted to go to...i got exactly out of the experience what i wanted. sorry to lack details but it was really mind numbing and ya know how hard it is to describe. i went to a beautiful place with truly good people who were not mad at all of me wasting the spice. it was truly beautiful...some of the best visuals ive evr seen. it lasted quite a while. i remember a lot of light relfecting off of metal type stuff. lets just say Alex grey did it a lot of justice but he just cant capture the motion and kaleidescope and the utter awe that it brings.
Posted 24 April 2009 - 02:08 AM
This is a pm i sent to someone so its not the official tek...he had asked my method for infusal. One day i'l prepare a finalized tek with pics etc.
absolutely! let me tell you ive told so many of this method and i dont think anyone listened but i guarantee if done right with some good Spice it will nail your ass to a cross...real deal man no joke! if your having trouble burnin it i feel ya i never figured it out.
So basically ive got this down to an art...always workin to get better but I under stand how to get it to crystalize on the herb properly.
Most important you have to get mullein..its the only stuff to use its so cheap online its ridiculous. when you get it try to use the fluffiest pieces and sift out all the stems in mine there were a lot.
Also as important bestine is the only solvent to use...i repeat the only solvent to use. pure n-heptane. IPA blows, acetone sucks, ive heard high proof grain alcohol works im guessing it doesnt because it has water in it which Spice cannot crystalize in.
OK, 2 parts Spice to 3 parts mullein. for example 500 mg Spice to 750 mg mullein.
It works best to use a pyrex shot glass. please do not use cheap shot glasses they break in the hot water bath...i know from experience. its sad to hear that crack and then 500 mg Spice going to shit.
if you had a standard shot glass it takes about 10 ml of solvent. you want about a ml or two more than what it takes to completely cover the herb.
OK, you have to heat bestine to about 130 to 140 F to get it to dissolve Spice . Do not heat anything over 140 F with freebase spice.
So id take a shot glass fill it with 10 ml solvent +/-. heat it first to 130 F then add the 500 mg freebase Spice and dissolve it, keepin temp below 140 but heated to dissolve it. once dissolved add in the mullein leaf. the solvent should be a ml or two above leaf
ok so now youve got the leaf sitting in the pool of solvent. take it off the hot water bath and let it cool for 5 minute, then stir it all up and let it sit and come to room temperature.
Spice in heated heptane as it cools to room temp will crystalize right before your eyes. you stir after five minute so the crystals dont all crystalize in one spot..you dont want big crystals you want a thousand little diamonds all over the leaf. after you stir you displace and break up all the first crytals then as it cools for the next ten minutes it crystalizes on the leaf. at this point it needs stirred...stir it up good. Now the solvent level should be a lil below the top of the leaf.
i place a small fan a couple feet away to speed up a lill bit in the evaporation..no direct fan just slight indirect air movement. it'l take about half hour to evaporate.
During this time its very important that when you stir like every 5 minutes you only fluff the bud. any bud on the top that is no longer sitting in solvent you do not want to resaturate in the solvent. Kepp fluffing it up and it should be simple. understand what i mean?
So after the solvents all gone you could either leave it in the shot glass to fully dry or you can just set it on wax paper or glass something flat that can air it out and let it evaporate fully. Dude you wont believe what it will look like if you do as i have told you. it will look like a thousand diamonds are on that mullein leaf.
OK, so now how to smoke it. also, very important. take about 125 mg of that infused leaf and pack it in a regular glass pipe. now direct flame destroys Spice so do not hold you lighter over the top. hold it so the lighter dips in over the side and it would be impossible to burn it all...think conserve the green. quik flashes with the lighter til you get a cherry goin. do not hold that lighter on there for more than a split second. quik flashes til you get a cherry goin take long slow deep breaths. 3 hits hold them i as long as you can. usually after the first hit itl have a small cherry still burnin and you dont even need a lighter for the second or third hits which is perfect.
If you use the lighter in short bursts and do it right you should smell nothing at all. If you burn it at all itl have that Spice smell. if you smoke Spice properly it will have no smell at all and light you up like you never thought possible!
ask any questions im sure i 4got sumthin but i think most of it is here it is all important! some is technique the rest if having the proper materials...good luck!
Posted 24 April 2009 - 03:08 AM
Posted 24 April 2009 - 11:44 PM
OK, the acid soak part was good. the only problem that i could see as what caused the excessive oils is the boiling. im not sure if maybe it brought more oils than spice. the decanting was much more excessive than the previous soaks. Honestly, after all my research i feel that citric(ascorbic) acid is the best to use for extractions. Phosphoric maybe to strong.
After reducing defats must be done. throw whatever you can at it naptha toulene xylene etc. Something must be done to alleviate the oils.
OK, basifying went well. now my recs to the pulls. i feel all fresh naptha pulls could have grreatly reduced the dirtiness. It seems that a fully saturated base solution the naptha can pull 1 gram/100 ml room temp naptha. so with expecting 1% or in this case about 9 grams 4 pulls equalling about 1000 ml(4*250ml) should get the initial 1% out. Remember no evaporation was needed to get the spice out. from previous experiments id say that 500 mg s remaining and could be freezed preciped out from each 250 ml naptha. however testing spice precipitated out after an initial precipitation is not strong...its dirty spice id say half pure(50 %)
1 sodium carb wash and one distilled water wash should be done on each pull.
I feel if extensive defats are done, and four fresh pulls that are shaking to hell and back and washed and freeze precipitated without reducing that you should be able to get 4 pulls, a 1 % yield, to all look like the one pull that looked like pure white from the pic in this tek.
This tek isnt done either. FASA pulls are being done and precipitated but the dude has been real busy to finish it up. Also, the first 2.2 grams of white has been converted to mullein infused leaf. 5 grams wasted thru recrystallization and there's about 3 grams from the final pulls that needs cleaned. he's going to do a FASA conversion to a salt, do acetone washes, then reconvert to a freebase to see if that is an effective means to cleaning oils.
Posted 27 April 2009 - 12:19 AM
Basically, do pulls with toulene(i prefer toulene over xylene bc xylene is god awful smelly...you get headaches when you work with it!) then salt with fumaric acid saturated anhydrous acetone. What comes out is beautiful long skinny cylindrical shape crystals!
Process is based on the fact that free base spice and fumaric acid are both soluble in acetone whereas dmt fumerate is not. mix freebase saturated acetone with fumaric acid saturated acetone and dmt fumerate precipitates out.
a good run thru on the FASA process...
OK, so 1.5 g of extremely yellow d was taken and dissolved into a minimal amount of acetone. it took 25 ml to dissolve. a few dirt and dust insolubles were quickly filtered out with a coffee filter. the freebase saturated acetone was piss yellow. about 450 mg fumaric was dissolved with acetone. about 50 ml of acetone was used to dissolve the fumaric acid. now when you add the fumaric acetone do it slowly and do not shake or stir, just lightly drop in the acetone. it was done in 10 ml increments. upon first salting the solution clouds up a lot but will settle will crystals after 10 minutes. after the 4th 10 ml was added it stopped clouding when the fumaric acetone was added that way you know its done. thats y you do it in 10 ml increments bc you cant tell when it stops clouding.
in this recrystal the dmt fumerate precipitated beautifully and the acetone remained piss yellow(thats the 2nd pic) and was poured off. i'm thinkin alot of the impurities stayd in the acetone. at least a good part of the yellow did. i mean check it out. im really impressed with this so far!
to be continued...
Posted 27 April 2009 - 12:39 AM
Ok, so check this out! you know when you scrape an evaporation dish or jar there's always that layer that just cant be scraped. over the course of an extraction these losses can add up. Well during the frezze precipitations etc there were about 7 jars that had a layer that couldnt be scraped with a scalpel. about 20 ml of toulene total was used to rinse these jars. freebase spice is extremely soluble in toulene(where as you can put freebase in naptha or bestine and it sits there) so it cleans them almost spotless. it grabs the oils to no big deal bc your just trying to be efficient. this 20 ml toulene which became very yellow was salted with fumaric saturated acetone and what resulted was quite a good bit. he didnt tell me how much but it looks like a lot. i mean these are jars that previously would have been cleaned and all that goodness wasted.
the salting went a lil dirty thats y i think it has the yellow at the bottom less thats some jungle but probably oils. this lil bit im guessing 500 mg fumerate will be quite useful. acetone washes and maybe ipa washes will be done to see if it can dissolve the oils without the fumerate.
Posted 27 April 2009 - 01:03 AM
Posted 27 April 2009 - 03:04 AM
Two 250 ml toulene pulls were salted with fumaric acetone. about 250 mg equiv fumaric acid was added to both. the crystals were removed and the toulene resalted. the first jar produced the whitest most crystals. it seems the jungle alks salt out first. this confirms a previous suspicion in my previous FASA salting thread. all were about 500 mg fumerate. i was expecting quite a bit more but .5 to 1 each 250 ml pull it is what it is.
the left most yellow snot looking stuff is the most interesting. it was my suspicion that the jungle alks salt out first and the first pull could result in the most jungle alks. what resulted was this waxy stuff. im not sure what it is, i dont think there is a good pic out there of the jungle alks in salt form. this could be them or this could be the oils i hear sbout when during salting the toulene gets agitated too much. he dont recall it being agitated any different fron the second jar.
you can see after the initaial salting of the 1st jar another salting was done. this resulted in the super white fumerate crystals you see. this color white should be the benchmark of what fumerate crystals should look like,
on the right are the crystals from the toulene rinse salting from previous post. these will be used to experiment to see if acetone washed or maybe ipa can remove the oils.
so the oils fromn the first two pulls im not sure if they are oils or jungle alks. they should be jungle alks but i believe theres ouls too so i gota figure out how to seperate them in salt form if possible. i remember a salvia purification thread that used xylene, ipa, water, and acetone in a particular order and it removed the oils. i believe with enuf experimenting it can be done or at least discovered it cant be done.
im extremely interested in that snot looking stuff. he may re extract with an a/b and do pulls with xylene. from there he can pull with xylene and then evaporate. it should be a super small scale extraction with minimal evaping. at least whatever it is will be freebased and could be tried out. in my experience in a hp extraction there is only about maybe a hundred mg of red...im not exactly sure tho. in the past if not successfully seperated the red in any quantity.
but for the recystal to have alredy removed almost 27% of impurities with out even being close to white it confirms that this is definately pulling alot more oils than a regular extraction. and any noticeable increase in yield could all be attributed to impurities.
Posted 27 April 2009 - 12:04 PM
but for the recystal to have alredy removed almost 27% of impurities with out even being close to white it confirms that THIS is definately pulling alot more oils than a regular extraction. and any noticeable increase in yield could all be attributed to impurities.
what exactely do you mean by "this"? using excessive water? using a wide array of questionable acids? not doing a defat?
if your dissin on using 'excessive' water Im gunna have to step in and defend her honor... :ballbat:, my last batch using wayyy excessive water (20+ gallons per kilo), ascorbic acid only, 3 hot toluene defats, 2 hot naptha defats, 5 hot naptha pulls, substantial evaporation, one freeze precip, and ONE recrystal got me a solid 1.2% yield of FLAWLESS glass spice plus another .1-.12% yield of really yellow spice on top of that, it dont look too pretty but it will form a stable solid at room temp and knock you to the grounnnnd if smoked. 1.3-1.32% total smokable yield, if its was ALL combined it would appear snow white. plus I have 3 hot toluene pulls done on the same solution after naptha pulls that i have yet to do anything with, who knows what could be in there. I propose instead calling this the "excessive water tek" it be called the "water tek" and other teks be called "insufficient water tek" haha jus kiddin, but seriously tho dont diss on the excessive water...
Edited by AndyLandy420, 27 April 2009 - 12:06 PM.
Posted 27 April 2009 - 02:41 PM