Extreme's Excessive Water Spice Extraction
Posted 09 April 2009 - 11:50 PM
The point of this was to test if using excessive water in the acid portion of an a/b extraction could significantly improve yields. Long story short before i go into detail...880 grams(~1 lb 15 oz) of mimosa was soaked with a total of 16 gallons of water and reduced to less than a gallon of water before basifying.
First off this dude wanted me to say that the acid portion of this was an insane amount of work that took over a week and a half to complete. 5 soaks were done. distilled water was used during the entire extraction. all soaks were let to sit the entire night to steep and eventually cool. Decanting was done before filtering out of the pot. a 22 L stainless steel pot was used. while heating it was stirred the entire time, the entire time.
1st soak - 4 gallons water, no acid, no heat.
2nd soak - 3 gallons water, 6 grams abscorbic acid, brought 165 F
3rd soak - 3 gallons water, 3 grams abscorbic acid, brought to 180 F
4th soak - 3 gallons water, phosphorc acid used to bring ph to 3, brought to boil
5th soak- 3 gallons water, phosphoric acid, brought to ph 4, brought to boil
Some details, when the desired temperature was reached the heat was turned off. the water took over 12 hours to cool each time leaving ample steeping time. after decanted the acidic mimosa soaked water was run through a cotton tshirt and let to decant an additional 24 hours and then run through a coffee filter. You can see what was left in the containers...mostly fine bark but with an oily texture. had this weird red film that was not water soluble.
The phosphoric acid soaks that were brought to a boil were a little harder to clean. an extra refrigerated decanting cleaned the fourth but even after two refrigerator decants the 5th still had a lil bit of cloudiness but was deemed acceptable.
Now why did he use different acids. he did so to test if using different acids could help in procuring more goodies. The first soak used plain distilled water to soak at room temp to get the goodies out without affecting their natural state too much. Phosphoric acid has been said to have great strength in pulling spice. The main reason abscorbic acid and phosphric acid were used which in his eyes was very important was the fact that they both have antioxidant abilities. Honestly he has no basis to say it could positively effect extractions and the reduction of oxides but since he was adding mucho heat and reducing so much he figured it wouldnt hurt. He actually doesnt pay much attention to all the mumbo jumbo about dmt oxide but just in case. Phosphoric acid for example works in rust removal by removing the oxide from iron oxide and making it iron phosphate.
Man he wanted to pull until the water came clear but it simply wasnt happening. after 8 gallons per pound it was still pulling color. You can see the 5th pullin the bottom left of one of the pictures. the third pull was still very dark. duaat said it could take up to 10 gallons to pull all the color and im thinkin shes underestimating. i bet after 15 gallons youd still pull color. not sure how much boiling had an effect on things. Most teks do not bring the bark to a boil. WARNING - stir the bark the entire time its on heat especially if bringin it to a boil. stuff burns in stock pots ask anyone whos heated spaghetti sauce in a restaurant...ya gotta stir the whole time. he never burned it at all...what you see in that pic is what precipitated after reducing. it was clean before it cooled.
after all the soaking and filtering and decanting he was finally ready to reduce 16 fucking gallons. Does anyone have any idea how long that really takes...about 32 hours at least of boiling, took 3 days with breaks for work and life and stuff! OK, so after all this was reduced to 3 liters it was allowed to cool so the insolubles could precipitate and did they ever. He coulnt even explain what it was at the bottom. It looked and felt like tar, had a lil bit of bark, some red crusty stuff. the stuff dried and could be chipped away and looked like bits of coal. this stuff was in no way water soluble so he deduced no actives were in it. hes not sure tho so hes saving that coal looking crap.
gonna take a break in the thread...up next basifying!
- August West likes this
Posted 10 April 2009 - 12:27 AM
Basifying was done with good ole NaOH, It was added in small amounts until the ph was 13.4. A note for other extractors...initially 70 g's was added to basify and it came to a ph of 11. I remember recent posts discussing the amount of lye to add to an a/b. I know some teks say 70 g's will neutralize the acid and be enough to bring the water to ph 13. this figure i figure does not account for the acidity of the bark which can vary and how much it buffers the solution. in total it took a half pound to bring it to ph 13.4.
Ok, now to the really good part and all of you out there you gotta check out what this dude did in one pull. Now even tho many of the teks out there say to not shake the mixture during pulls but it needs to be done. hes done it many times in the past and if the solution is basified enough everything will settle to two perfect layers in less than 5 minutes. But, before doing the experiment he felt that even tho he knows excessive shaking greatly improves pull yield he wasnt sure if it pulled any extra impurities.
So...during the first pull! By the way 250 ml room temperature pulls were done with Vm+P naptha. the first pull he did not shake violently at all. for a half an hour he lightly swirled the mixture making sure to not cause much aeration etc but he did full swirl it completely if ya know what i mean. the second pull the mixture got the evin livin shit shook out of it for a few minutes then repeated a few minutes later. he let it settle for a few hours before pulling.
To each of the pulls he did a 30 ml sodium carbonate wash(ph ~10.68) then proceeded to do a 30 ml plain distilled water wash.
Ok, so here's where it gets really interesting. He placed the two pulls into the refrigerator for a few hours then the freezer for most of the next day. the second pull in the refrigerator after less than a half hour started precipitating
crystals, in the freezer it went apeshit. the first pull didnt do much! He did not evaporate any solvent before refrigerationg nor did he add heat in any way to the pulls. the base solution was even allowed to react completely before pulls were done.
the first pull precipitated nothing from the solvent except a few small crystals that wouldnt amount to anything. the second pull alone pulled fucking over 2 grams! did you hear that ~2.2 grams from 1 250 ml vm+p naptha pull done at room temperature and freeze precipitated without reducing.
O and the quality...these are cleaner than any crystals ive ever seen him produce before. I saw it in a pic next to his cleanest crystals ever and i cant believe theyre brighter and cleaner.
He had remembered reading in older freeze precipitation teks to freeze out the spice then reuse the naptha. He felt that in previous extractions that by reducing the naptha first he was exposing it to i guess oxidation. he was also using a heated fan previously and has since learned this definately causes a slight diswhitening of the spice.
he reused the naptha for the 3rd and 4th pulls and thay both were shakin to hell and back and both precipitated crystals after a half hour of being in the refrigerator. So il leave you guys with this and tell you the rest of the story another nite...sweet dreams!
Posted 10 April 2009 - 12:50 AM
Nice work man
got a total yield?
- Shadowlord likes this
Posted 10 April 2009 - 01:00 AM
Great work Extreme.
You are the mad jester chemist indeed.
I hope to get half as good as you are at it!
I have to give out some more rep b/4 I can hit you again but here is a Rep I.O.U. :thumbup:
Posted 10 April 2009 - 01:02 AM
Posted 10 April 2009 - 01:10 AM
I have to give out some more rep b/4 I can hit you again but here is a Rep I.O.U. :thumbup:
Posted 10 April 2009 - 05:31 AM
Posted 10 April 2009 - 07:29 AM
(PS: have yet to do a STB on the junk bark)
Posted 10 April 2009 - 01:55 PM
Posted 10 April 2009 - 02:06 PM
Is he going to evaporate the solvent when he's done with it?
It would be interesting to see how much spice if any is left after a freeze precipitation.
Posted 10 April 2009 - 02:13 PM
he's sure those two cups of naptha would precipitate more if evaped down just will do so when he can clean the house etc so its not so nerva racking.
he's gonna pull til the cows come home. because the second time using the naptha the pulls were much more yellow for the 5th he used fresh. After that he'l do heated pulls which should definately yield a good amount to. after that toulene to pull with FASA precipitation.
the yellow isnt that big of a deal a recrystalization will be done on anything discolored.
but over 2 grams per pull without using heat or evaporation is wonderful!
Posted 10 April 2009 - 02:53 PM
What do you mean your not evaporating any solvent and not using heat?
Posted 10 April 2009 - 03:00 PM
also most reduce the volume of thir pulls before freeze precipitation to reduce the amount of solvent that can hold the spice. it helps by saturatng the solution to ease the preciptation of crystals.
Posted 10 April 2009 - 08:22 PM
Posted 11 April 2009 - 11:08 PM
pull five fresh naptha still room temp - 1 + g yellow
pull six and seven- 1 fresh 1,1 reused naptha...odd the one with fresh netted nothing and the 7th pull reused netted another fat 1+ g.
So far 1 % yield which aint bad i guess the problem i see is how yellow everything past that bright white pull is. i mean the yield is good for this type of extraction. Let's just say when he did the normal marsofold style tek he yielded like .86 and now he is over 1 % but the quality and color is just yellow past the first 2 g's.
to note in dpwishy's thread he yielded only about .13% more by doing all the additional acid pulls on the spent bark. the additional yield of this tek is right on par with that.
the heated pull was full of oils especially.
One very important note. No evaporation of solvents was done at all. no smell in the house at all he said. I cant underestimate the importance of this. I think by having the solution so saturated it was able to pull the max amount naphta can pull which as i figure is about 2.2 g per 250 ml. oddly another thread recently had this same figure. it was able to be freeze precipitated and crash out 2.2g/250 ml without reducing.
this said he does have a liter of solvent that is probably holding a lil bit of spice which probably at some point needs to be evaped down and re freeze precipitated.
I think 2.2 g/250 ml pulls is the figure we should be aiming at for each pull. A very important thing learned. shake the living shit out of it when you are doing your pulls. It has no effect on the cleannness of pulls and the difference as seen in the first two pulls was 2.2 g. the first pull lightly swirled yielded nothing where as the second pull that yielded that snow white beauty was shakin to shit and back.
so this dude took 5 grams of the nicest yellow spice he had pulled and using andy's cooler recrystalization tek hes attempting to clean it up. hes keepin me in suspense as to how it turned out. gota wait til i see him again. if you dont know what that is he took 5 g's and dissolved it into 150 ml bestine and heated to about 155 F. he had waiting a cooler filled with 6 gallons of 155 F water and placed his vessel containing the solution into the cooler. the idea is its gona take that water well over a day if not more to cool off. at some point the impurities are going to crash out before the spice and collect in a corner at the bottom. the now clean dmt solution should begin to crystalize as it becomes cooler and if all goes well should be a sight to see.
Posted 16 April 2009 - 04:33 PM
Ok, so thoughts on using excessive water to extract. well. il say that this is the best yield hes ever gotten its also the dirtiest. The additional water pulls more oils than spice i believe. these are tricky oils too. they're not so easy to seperate out.
Maybe it would be worth using twice as much water as the teks call for and it was advantageous to boil down the acid phase to a more workable amount but the fact is the additional weight pulled was all impurities. Like this is some yellow shit past that first good pull...few nice ones here and there but oil oil oil man.
i'l also state this in dpwishy's thread he said the additional acid soaks produced clean spice so take it as what you wish.
- director of sound likes this