right now im doing side my side of two source materials, once i get that done i could do a 20g a piece of the higher yielding source, but even then im going to pick the highest yielding means and then add everything together to get out ever last drop.

i understand what your saying, a side by side profile would be of considerable value, it would give good reason to justify making the salts a standard of the process, but for right now i just want to get this experiment done first, ill be decanting it tomorrow.

also side note to all this, you dont need anywhere near 70g for 300 ml of water once all the bark has been proken apart by acid, at half that ammount the salt was falling to the bottom, but thats what this process is for.

ok i got good news and strange news

first the good news

subject 1: 480+/-3mg first pull
subject 2: 472+/-3mg first pull

now i tried to do it a second thime but this time i decided to shake the bottles rather then turn them end over end.

they have emulsifed and are not coming out even after a day.

i can see the solvent but its not moving at all.

what can i do to fix this?

thank you

_______________________

Edit:


found an answer by putting the entire jar in a water bath at sterilizing temperatures.

thank you ancotar.


i should have the results in a day or two, its looking good.

ok im putting this on hold for a few days i just got the bajebus scared out of me.

i dont know what happened so ill just recount the events.

demulsified the goop, everything was going great, shook it again for round two and it decided, even with the warm bath, not to come out of suspension this was the same for both bottles.

opened one jar and looked inside seemed ok just not doing anything at 80 celcius, i took a look at the edge and say a layer of solvent bubbles half way up the jar side then i took a glass stiring rod and decided to swirl it around.

the thing was super heated or super emulsified or something, immediately the solvent started all rising to the top at once, few second later something appeared to rise out of the goo that didnt look like the solvent or the goop (or the magnesium sulphate) and then went back under.

few second later the entire thing cracked open.

i cleaned it up and when i went to the other jar (which was outside of the bath) it had fully emulsified, i pulled the solvent and im sitting on its precipitation not five minutes ago.

i dont know what happened, like i said maybe the thing got super heated (i kept it at a steady 80c) and decided to spontaneously demulsify, but im putting this on hold for a few days.

First of all, what is Subject #1, and what is Subject #2? Are they both MgSO4 extractions, one of them? One NaCl one MgSO4? neither?

Here's the thing. It's possible the magnesium hydroxide is making the emulsions a lot worse. It's not particularly soluble in water and I can't find much information about it's solubility in organic solvents. likely it would have an incredibly low solubility in them. That doesn't mean though that it wouldn't form weird micelles or something at the bi-phasic interface.

So you observed no emulsion with only MgSO4 water and sodium hydroxide with naptha? I may recreate this experiment with say a drop or two of glycerine or vegetable oil to simulate plant fats.

You still were not clear as to whether the control experiment was evaporated or not.

Do magnesium hydroxide emulsions exist? They most certainly do.
http://www.drugs.com/uk/...emulsion-bp-leaflet.html

The thing with emulsions is they are typically not one component. So maybe the water, Mg(OH)2, and naptha alone won't cause trouble. However with the addition of plant oils and such they very well could form a vicious emulsion. Hard to say.

or maybe you're just getting a case of the unlucky emulsions and I'm over thinking it.

hello inmotion

source 1 and 2 are two different resources of mhrb, one being a prepowdered, the second being a bark i powdered myself.

there is no control im just trying to reproduce what happened the first time.

what i observed was at room temperature nothing happened, but when i then put in a glass rod and swirled around the mass the entire jar spontaneously emulsified which means a layer of something formed which trapped the naphtha, then as i recounted something appeared in the middle of the jar which had a different refraction index then the solvent, got to the top then fell back down into the black goo and shortly after the jar shattered.

the one thing im wondering is if water with epsom salt is heavier than water without (most likely) and if it is possible for it to trap the solvent, either all on its own or under a layer of lighter water.

also good news from the second pull from the jar that did not shatter open

second pull produced 190mg from source 2 (the bark i had to shred myself)

combined with the first pull thats 670 mg divided by 25g

2.68% from two pulls (but i was suppose to do four pulls, but the main interest is that source two was the new source i was using for comparison, so the numbers so far are looking promising)

im slowly getting better at this and another 2 jars of bark was put into the freezer not a half hour ago so im back at it.

this time im going to more accurately reproduce the effects of the first test and use a combination of magnesium sulphate (for its ionic effects) and sodium chloride (to break up the emulsions) so i dont have the spontaneous demulsion occur again and pray the gods of extractions that they will bless me with similar results to the first experiment, and then once that is done i can apply occam's razor and refine the method.

next time though, im not going to heat the jar to 80C, thats for sure.

thank you everyone

hello everyone

im going to put this on hold for a bit until i can find a safer way to do this.

in the last month i have done 2 attempts (4 jars total) and had another spontaneously de-emulsify. fortunately instead of a jar breaking open all that happened was that the lid went flying off and it started spilling over the side into the pot that i put the jars in case the jars cracked open.

the interesting thing is that the jar was not any warmer than the other jar, so there was no exothermic reaction, but something is causing all the solvent and all the air bubbles from shaking the jar to become trapped and then release all at once, and i need to figure out why this is happening and find a way to stop it.

if anyone has any clue what is happening or how to stop it please let me know, i have only had 2 out of the last 9 jars do it, but thats still a pretty high number.

just speculating, not the heavier magnesium saturated water seperates from the non saturated water, and then a dome of powdered bark froms on top of it, just enough to form a net for the solvent.

from there the air bubbles become trapped either inside or under the solvent and when something happens, (like a hole opens up in the layers) all the solvent and air jumps out at once.

this maybe be as simple to fix as stiring the jar regularly, or using a bigger jar, or using a mixture of table and epsom salts (something i have not tried yet and need to) or any of a number of other things, but i honestly dont know what is happening.

that said the results from the first two jars of four came back

after four pulls of 25g

jar 1 pre shredded 690mg, 2.76%

jar two whole bark 720mg, 2.88%

i still think with a combination of salts this could be pushed even higher, but without a better understanding of how to stop that bubbling problem i'm very skittish to keep trying.

so if anyone can provide any insight into what might be happening, please.

thank you.

hello

quick update

i have been running down reasons for what has been occuring and found something interesting.

there is a type of natural disaster that causes all the gas inside a lake to spontaneous come out of suspension, i dont know how much this has to do with what happened, but the information i could find about it was extreme limited, but it matches somewhat to what is happening to some of my jars (only on a much larger scale and with no carbon dioxide)

im putting this out hoping someone can find some information about this and possible a term for when it is occurring in a laboratory setting, (and hopefully a means to avert it). im guessing this would not be something wanted while in a sterile environment but this is the closest i could find to what is going on.


thank you.

hello

ok im resurrecting this thread because i kind of made a breakthrough and i need someones help for outside verification.

those limnic eruptions i mentioned, the spontaneous decanting of the solvent when with slight agitation everything would separate out into layers (with bubbles and flying goop) was a very scary thing, but i found out the reason for it.

magnesium sulphate saturated water is heavier than sodium chloride saturated water or water that was not attach to any salt

the tannins and bark seem to have a habit of settling on top of the magnesium sulphate saturated water, in essence creating a barrier (or a net) which would trap the solvent, when the net broke that is what caused the eruption.

i have figured out three ways to get around this problem

the water must be completely saturated with only magnesium sulphate

acid baths

the solution needs to be regularly agitated while separating (or place in a self contained jar) so that the layer which, if it forms on top of the magnesium sulphate solution, can be broken apart.

now at this point i need independent criticism and experimentation, particularly with someone who has xylene or toluene (since i dont have either) because that should increase yields significantly.

based upon what i have done it is possible to get 1.3-1.4 g from 50g of bark (based upon the two source materials i have) but with the broad spectrum solvents that number should be able to go up.

and i repeat to anyone who does help, that problem of material forming on top of the solution and trapping the solvent i have not entirely been able to stop (except with acid bathing the bark and then using the resulting bath alone) so please use caution.

now the proto tek:

50g of mhrb

take 210ml (20ml per 1g + a bit extra for good measure of evaporation) of deionized water, bring to below to low simmer and proceed to pour in desiccated magnesium sulphate (remove all the water from the magnesium sulphate prior to pouring it in so it will full bind with the deionized water) into the solution until no more will saturate.

take 50g of mhrb or acrb and pour it into the saturated water, than add a small amount of acid (10ml of vinegar should work, i used some citric acid crystals) and let everything get thoroughly mixed together at low heat.

jar the entire concoction and put it in the freezer for good measure.

pull out of freezer after solid and put the jar in a warm/hot water bath

once it is liquid again leave for a few minutes and then open the jar and examine if a layer of bark forms on the surface by taking a stick and skimming the surface (this is the barrier i keep warning about, this is just for precautions for later) if it is absent then great, if present then its still ok, just dont open the jar when your at the solvent separating stage until you can clearly see the layers

take the jar and add a bit more magnesium sulphate and acid in for good measure then bring it to another simmer, regularly stiring.

now let it cool down to room temp then proceed to take 5 table spoons of lye and add to a minimum amount of water (not the other way around) too saturate and pour in.

once the solution is alkili proceed as usual with pulls, if you can doing it while still as warm to increase the solvents pulling power. pour in solvent, agitate as if it was a salt tek (emulsions are non existent, also the magnesium sulphate and lye do not combine to make milk of magnesia, or if they do they dont get pulled by the solvent so dont worry about that) and wait for it to separate, if after a short period (10-20 min) you do not see the solvent exasperating pick up the jar and give it one single hard shake, you should when you put it back down literally see the solvent pouring up and out of the solution (DO NOT OPEN THE JAR TO OPEN AIR PRIOR TO SEPARATING, THE SUDDEN DECANTING CAN CAUSE THE ALKALI SOLUTION TO MOVE QUITE A BIT SHOULD IT OCCUR).

and with any luck, a person using toluene/xylene should be able to obtain at minimum 1.4g+ (which is what i have been able to achieve with naphtha.

to anyone who does help out with this thank you, please be careful and if you find something going wrong let me know.

good luck


tl;dr

0) be careful, wear all the protective gloves and goggles, keep vinegar nearby to neutralize spills (SPONTANEOUS DECANTING OF SOLVENT CAN OCCUR, DO NOT OPEN THE CONTAINING JAR IN STEP 9 MORE THAN SLIGHT TO RELEASE GAS UNTIL THE SOLVENT HAS COMPLETELY SEPARATED)


1) 210ml deionized water brought to 60c.

2) dessicated magnesium sulphate is added until solution is fully saturated.

3) 50g of bark is added alone with a small amount of an acid (10ml acetic acid, 1g citric acid exc enough to just tip it towards slightly acidic).

4) let it simmer for a half hour stirring regularly.

5) place in freezer till hardened.

6) thaw and add a small amount more acid and simmer for another 30 min.

7) transfer to self contained jar, saturate 5 table spoons of lye with the minimum amount of water, pour lye solution into magnesium sulphate solution slowly, regularly stirring.

when cooled enough to handle from reaction, pour in solvent, agitate and let sit.

9) should after 20 minutes the solvent layer not form, give the container one good shake to break up possible net of debris trapping solvent, the solvent should begin pouring out of suspension (DO NOT OPEN JAR UNTIL SEPARATION HAS FINISHED).

10) retrieve solvent pull and proceed to precipitation.

11) when all alkaloids are fully retrieved, acidify magnesium sulphate solution to near neutral ph and dispose of properly.

12) please share any insights you find, the totals retrieved and please be careful.

I don't think you're getting very much response from this because the process seems extremely dangerous and no one wants to take that kind of risk. I wish the epsom salts did not cause this type of reaction because it all actually seems quite promising. I would not even dare attempt this method even if it did reach 3% or even 4%. I don't think very many people want to take the risk of having their stuff explode.

MgSO4 + NaOH...

http://answers.yahoo.com...id=20100311172139AAS2zhS

thank you for the input and yes that is why i warn about this early on and repeatedly.

it does not explode, all you have is a trapped layer form under a mesh of plant material resting on top of the magnesium sulphate water, it is something which needs to be addressed and i am doing which is why i took a half year between posts, the risk only goes down by working through it and figuring it out, this will probably have to be an a/b tek where as little plant matter is in the jar for the final steps, but thats why prototypes exist, i want to fix the bugs, but at the same time i want anyone who does help out know what happened.

all that said, when i have used a through acid bath and use the resulting bath for extraction that this spontaneous decanting does not occur, but its one of those situations where better safe than sorry and i need more information, that is why i am asking for independent analysis from someone who has a solvent i do not.

@dooby the question of producing milk of magnesia has been asked and mentioned repeatedly and i have tested it, even trying to make it at home (using magnesium sulphate saturated water and pouring lye saturated water into it).

the result is that i was unable to make milk of magnesia when i tried this (which was as close akin to how the process in general would occur) and when naphtha was poured in to a bottle of pure milk of magnesia with water bought at a store trying to extract the milk, it would non suspend in the solvent.

so even if milk is precipitated it will not contaminate the results. (as far as i know, maybe xylene or toluene can pick up milk of magnesia, but i have been unable to do it with naphtha)

Are you purchasing anhydrous magnesium sulphate? If you are dehydrating it yourself, why not just skip that bit entirely and add the heptahydrate to a smaller amount of water? The correct volume is easily calculated although I haven't bothered to do any of that yet.

A probable reason why this technique seems to work is that the magnesium will be displacing the alkaloid from its tannates. This speeds up the extraction process - hurrah!

IMO the anhydrous magnesium sulphate bit is a waste of time and effort not to mention the fuel bills if you're roasting your own. Just use it straight from the tub as heptahydrate and use less water. Where I live, pharmacies and health food stores sell massive tubs of the stuff, pharma grade, for not very much money, presumably you know this already (except, hopefully, where I live )

i got a giant bag of it, many many kilos, dehydrating the magnesium sulphate may not be neede, it just seems like a good idea, but if it suspends in the liquid at the end of the day thats all that matters.

on the same note as this on the question of ions, would running a current through the goop increase the electrical ions inside of it (thus potentially increasing yield)?

there would be a whole other matter to getting the solvent to pick up the alkiloids inside an electrified goop but i wanted to ask if there is something fundamentally wrong with the idea of increasing the ionization by an electrical current?

the one thing interesting is that if i understand it, magnesium sulphate saturated water is extremely electro conductive, so i thought it would be worth asking.

Why does it seem like a good idea? You are just wasting loads of energy removing water and then putting the magnesium sulphate into... water!!

I don't recall if this has been mentioned earlier in the thread, but I just noticed that adding a load of magnesium and sulphate ions also increases the ionic strength of the aqueous phase, which in turn should improve the partition coefficient of the solvent extraction. From this thread

I've just had another thought about the use of anhydrous Epsom salts: the hydrated bark will be subjected to a much greater osmotic shock from the higher concentration that can be achieved using this. There could be something to this - more than one aspect to it as well... It becomes a question of what you think about using more energy roasting magnesium sulphate to get higher yields more quickly versus taking more time and possibly less energy to get... what? Of course, if you use a solar oven, the energy footprint doesn't matter! B)

That's why he originally started doing this, I believe. And during his first attempt he noticed peculiar effects of the epsom forcing the dmt into the naptha at super saturated levels regardless of heat. It seems extremely promising, and dangerous.

Late night brain putty, I now realise! I've re-read the entire thread and on consideration I'd say once more that this technique looks very promising. One should always wear PPE (goggles, gloves, etc.) when using caustic soda, so while we shouldn't downplay the possible 'belching' hazard that sometimes occurs, nor should we overstate it. It appears that with due care this effect can be avoided. That's part of what being careful entails.

In addition, it may be worth mentioning that magnesium hydroxide is still quite alkaline, just not very soluble at all - "one part in 50 000 parts of water" according to my source. It also mentions that "in the presence of ammonium salts it is not precipitated as the sulphide, hydroxide or carbonate" which may be of some relevance. It could well be worth looking for evidence of complex formation between the spice N atom and magnesium ions...

hey guys

thank you for the dialogue i really appreciate it.

i should mention that doing this i have ended up with a good sized jar of red "jungle spice", but the thing that is drawing so many lines for me is the question of if a broader spectrum solvent will increase the yields im already seeing, as it stands its just under 3%.

their is a very real possibility that the ionic strength is high enough that it is forcing all the alkiloids that want to get out of the goop to do so, compelling them more forcefully than originally intended, but one of the other things i have been wondering about (and i think the conclusion is yes) is that freezing or boiling the bark while acidic with the salt in it also increases the totals.

this is one of the points where my understanding of chemistry and ionic strength fail, because i dont know if the ions are "pulling" the alkiloids out of the bark so that they attach onto the molecules with the excess ions on them or are "pushing" them out of bark and making them clump together, the reason i bring this up (and i need to be clarified on this) is that if it is "pushing" everything out, what i would have to wonder is what else would be being pushed around, besides the alkiloids, which may or may not be being picked up by the solvent.

from here comes the idea of using an electrolysis machine to increase the ion levels artificially, i dont know if it would be possible to get the alkiloids to "plate" onto a surface much like gold plating on jewelry (or if you could just force them into the solvent this way while in an inert enviroment) but this is the next step that will need to be examined once a conclusion is reached on wither a broader spectrum non polar solvent will capture more alkiloids than what is currently being found.

oh a side note to all this is a whole other strange question, does anyone know what added zinc dust (to act as an oxygen scrubber) to a solution would do to its ionic strength? i think this may be another avenue of increasing results as well given that nn-oxide does not bind to naphtha (but supposedly does bind to xylene and toluene).

my apologize if this message is long and convoluted, but now that i know what was causing those "limnic eruptions" to occur and how to control them, im just posting everything that has come to mind over the last few months i have thought up, hoping that all of this stuff can be answered in some way.

in short im starting to wonder if the ionic strength plays a much larger function than previously though.

thank you.

I don't know if electrolysis work on NPS. I don't think it conducts electricity very well. Don't hold me to that though. But even if it did, I would be worried it would catch flame. But then again I don't know the specifics of how electrolysis works.. lol

I think a narrower spectrum solvent would help you figure things out better than a broad spectrum.