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FASA - lost over 50% yield AGAIN

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blue.magic

Rising Star
I used 300 mg of very pure (recrystallized) DMT. I followed the FASA method from Wiki to the letter. The only exception was that I washed the DMT fumarate with fresh acetone several times (always let the fumarate to settle and decanted the supernatant liquid) to remove any excess fumaric acid and make sure the result will be DMT fumarate only.

And still I was left with only 176 mg of DMT fumarate, that is about half of the original weight of DMT. Since fumarate is heavier than freebase, I expect to still get around 300 mg of fumarate even when losses are present.

I am really tired and a bit angry. Why am I losing so much product every time?? I am not sloppy and tried the method several times, gone through tutorials on analytical methods and did everything to prevent losing HALF of the product. For example:

- prepared fresh anhydrous magnesium sulfate
- prepared fresh anhydrous acetone
- oven-dried absolutely everything (including bottle for the anh. acetone)
- flame dried every piece of glassware before use

Yet every time I make DMT fumarate using the FASA method I somehow lose over 50% of DMT.

How do you make DMT fumarate and prevent these huge losses and what could went wrong?

I am getting hopeless, checked and re-checked every step and still every time I work on my DMT, be it purification or FASA, over half of it simply disappears into nothingness...
 
Why don't you switch to FASI instead?

Sounds to me like your tone was not fully dry in the first place. Maybe you should have dried it more times with fresh anhydrous mag sulfate?

I'm reading your posts and concluded you actually encounter some hiccups lately. I know it can be discouraging, but try to change your methods.

To me it seems that your tone is either too wet cause it has a high % of water, higher than you expect, or it absorbs humidity from your environment very fast making your process go south. Are you evaping the tone over a fan maybe?

Using IPA ime, rarely causes such mishaps. It's also easily available almost dry so you'd only need to dry it once in the case of high purity one (even when they say it's dry it is still good to dry it yourself and make sure)

That aside, if you kept all materials and discarded nothing yet you can still retrieve what's lost.
 
I have distilled the acetone TWICE (with a fractional column - the vapor temp never exceeded 70 C and no, acetone does not form an azeotrope with water) and dried by excess MgSO4 which itself has just been oven dried for 2 hours on 250 C (which is excess by some standards).

I watched several videos on drying solvents and the magnesium sulfate didn't event clumped in the pre-distilled acetone so it was already pretty dry!

I have used FASA since this is a Tek in Wiki and thus it should work, doesn't it ??

Sorry for sounding rude but I just spent two days preparing the drying agent and drying acetone, drying glassware and being super paranoid about dryness. And now you say it's wet...

And by the way I did FASA on acetone intentionally slightly mixed with water and the result was the same. So either FASA does not work, or my 99.98% fumaric acid is not what it says or... I don't know. It enrages me as the tek sounds super simple and everyone else seem to have not problem doing it with much simpler equipment and just a store bought acetone.

I changed my methods three times already, I tried three purification methods and the results are always the same - significant loss of product.

Unfortunately at the time of realizing there is a loss, the amount of used acetone was over 200 ml and I don't want evaporate that much of (for me, precious) chemical.

Yes I failed several projects: 3 kilos of mushroom substrate have rotten, I lost half of harmalas after purification mistake, then I lost gram of DMT by accidentaly spilling naphtha beaker, and then this...

I don't want to try other methods. I want to know why this one does not work while it should and what am I doing wrong. Otherwise I will never understand some hidden mistake that is not mentioned anywhere.
 
Did you weigh your fumarates before the washing? What did you do with your acetone from the washing? Evap it and see what you get.

Lesson nr 1 is always "dont throw anything away until you're totally finished and happy with the results"

IME acetone wash should be cold too, at room temperature it may be a small amount of fumarates dissolve in it, and if you washed it "several times", there may be part of your loses.

Second option is that more fumarates were still uncrashed in your FASA. How long did you wait before retrieving your crystals? Did you try adding more FASA to see if it clouded up more? That could be another place where your DMT is.
 
endlessness said:
Did you weigh your fumarates before the washing? What did you do with your acetone from the washing? Evap it and see what you get.

Lesson nr 1 is always "dont throw anything away until you're totally finished and happy with the results"

IME acetone wash should be cold too, at room temperature it may be a small amount of fumarates dissolve in it, and if you washed it "several times", there may be part of your loses.

Second option is that more fumarates were still uncrashed in your FASA. How long did you wait before retrieving your crystals? Did you try adding more FASA to see if it clouded up more? That could be another place where your DMT is.

Yes there was a lot of fumarate but the amount lessen after acetone washes. I thought these were impurities.

DMT fumarate is said to be completely insoluble in acetone. How could the wash, even room temp one, could possibly dissolve it??

What bothers me most is that these extremely important hints are not mentioned in Wiki (e.g. use ice cold acetone, wait at least xx min for precipitation etc.). On the other hand, it even claims "100% recovery", but this is clearly BS. Someone should update the Wiki article...

I have also read "SWIM's Psychedelic Cookbook" and the author also provides the same simple steps and does not mention any of these little details (acutally super important) making me think FASA method is simple and straightforward and there should be no issues along the way.

BTW I don't retrieve any "crystals". It's a powder. Adding FASA and mixing creates a snowstorm effect and the "snow" settles. There is no crystallization.
 
These "important hints" are mentioned in the forum topics blue.magic! I think you can't blame the WIKI for your mistakes, sincerely.

Also you might want to tone down your language and continue in a constructive, civilised manner. I get that you're frustrated, but after all isn't chemistry the science of experiments?
 
Nereus said:
These "important hints" are mentioned in the forum topics blue.magic! I think you can't blame the WIKI for your mistakes, sincerely.

Also you might want to tone down your language and continue in a constructive, civilised manner. I get that you're frustrated, but after all isn't chemistry the science of experiments?

Well I spent many hours on the forum (about 30-40 minutes a day) over the course of years (last year actively) but never stumbled upon all of the little puzzle pieces. Some "gems" are buried deep down in the old threads.

I thought the Nexus works in a way the best stuff and findings of the forums are distilled into the Wiki, which will provide "The Official Golden Standard (TM)" methods and teks so one does not actually have to go through the ordeals of experimenting and repeat the same mistakes again.

I don't think reading an entire forum from start to end to collect all the little pieces is possible and viable.

For me it's a try-fail method, but that's okay. What enrages me is that I have to lose so much time and money in the process that it will never pay off in the future...

For example, some friend wanted 10 doses of Pharmahuasca for a healing ceremony. So I started working on it month ago and still can't get together more that 400 mg of DMT fumarate and then the friend lost interest because I was too sluggish in my progress. I would blame myself but I did my best. And it's not enough...

Now it seems easier to just get a 3 year chemistry course and THEN get back to experimenting. It will simply save the time in the result.
 
DMT fumarate is very soluble in water.
I don't know how dry your acetone was initially, but it is hygroscopic and takes water from the air even after drying with magnesium sulfate.

^^ Here it indicates to use cold acetone, not that hard to find 😉

Cold acetone and/or cold MEK washes are a bit of a standard.

Maybe you are protected from giving the "10"? Whatever happens there could easily trace back to you. Be careful please.
 
I hate to be mr. miyagys barking dog but feel there are some important things to outline here.

The FASA subforum consists in its entirety out of 242 threads, out of which only ±30% are quality posts. Not alot if you ask me. He who wishes to study this process can carefully study this subforum in just an amount of days, extract the quality topics and work with those as necessary. Of course that in order to thoroughly understand some of the processes one would have to study the theories, study accomplished and failed experiments by others, envision his own experiment, and only then put it into practice. Diving right into practice and trying to grasp things on the go is a no in my book.

Of course I understand that you have some chem background and maybe not all the above apply to you in particular, but I do have a feeling that you are more versed in theory than in practice. And I'm saying this because I've seen some of your last posts, issues related, and truly I can hardly believe you're unable to resolve some of them on your own.

For me it's a try-fail method, but that's okay. What enrages me is that I have to lose so much time and money in the process that it will never pay off in the future...

For example, some friend wanted 10 doses of Pharmahuasca for a healing ceremony. So I started working on it month ago and still can't get together more that 400 mg of DMT fumarate and then the friend lost interest because I was too sluggish in my progress. I would blame myself but I did my best. And it's not enough...

Now it seems easier to just get a 3 year chemistry course and THEN get back to experimenting. It will simply save the time in the result.

...about this bit

It is well known that trial and error are things to be embraced in the process of learning especially here at the nexus. Don't expect to learn without failing cause that's never going to happen. Embrace the process as a whole. Also experiments failed by others can provide good learning material, to me that's the beauty of this open source platform. I rather have access to every type of tryout by every individual than be restricted by just a couple of methods and outcomes... the rest I can handle myself.

Word of advice: don't look at these things to simply "pay you off in the future". Apart from the fact that numerous wanted and unwanted meanings can be subtracted from that bit only, you forget how rewarding everything you learned here actually is. Rewarding, a much better term than payoff. And honestly, I'd forget thinking about that ¢a$h too often... in fact I can't see much of a loss really, what's important here is that you have fun..

Providing tools as a means for healing others sure it can be nice, but I can't agree, neither with how you word it, neither with inoculating such expectations about you in others. It's wrong and unfair because all the process involving these sacraments is healing. From not knowing to the discovery of a total new way of life. Why would you take that privilege away from someone? Might aswell send them to church to meet god! I wouldn't have commented here if this thing wouldn't have reached the surface more than once on the forum...

The nexus is here for a reason and until now I see that it doesn't fail to deliver for those receiving the call. Your friends might aswell comply too..

Conclusion? People have the tendency to overcomplicate simple things. Sure, taking a couple of chem courses can be practical overall, but it's not like alotta people with 0 chem backround haven't succeeded to integrate the informations here and get satisfying results in the past. On the contrary, you'll find more self thought chemists here than academic ones, and I bet many learned a lot while being here.
 
blue.magic said:
I have distilled the acetone TWICE (with a fractional column - the vapor temp never exceeded 70 C and no, acetone does not form an azeotrope with water) and dried by excess MgSO4 which itself has just been oven dried for 2 hours on 250 C (which is excess by some standards).
Pure acetone boils at 56 degrees centigrade (Celsius). If you distill acetone, over a fractionating column even, and you collect any distillate that comes over at a temperature higher than that, you're not doing it right.

How sure are you that your "acetone" is really acetone? Suppliers do make mistakes occasionally. Methanol, various mixtures of methanol, ethanol, ethyl acetate and acetone could distill below 70 degrees and might cause the partial precipitation that you got.

I have done this procedure myself a few times using dried and distilled technical (hardware store) acetone and I mostly got nice needles after a night in the fridge. The only time when the result was powdery was when I used a mixture of dmt and nmt from an acacia extract.

blue.magic said:
I watched several videos on drying solvents and the magnesium sulfate didn't event clumped in the pre-distilled acetone so it was already pretty dry!

I have used FASA since this is a Tek in Wiki and thus it should work, doesn't it ??
TEKs in the wiki are generally presumed to work and if they don't, there would have been a flurry of complaints. Since this seems not to be the case in general, I would dare to say that the information in the wiki tends to be trustworthy. There are no guarantees whatsoever, certainly not with regard to operator errors, which have not been rigorously ruled out in this case.

Also be aware that nobody gets paid here to provide valuable information. Nor have you paid any money for anything (that I am aware of - in fact, wasn't it you who was soliciting donations for writing teks?) The only one paying for this site is The Traveler (and some gentle but unnamed donors.)

blue.magic said:
Unfortunately at the time of realizing there is a loss, the amount of used acetone was over 200 ml and I don't want evaporate that much of (for me, precious) chemical.
Since you appear to be in possession of a still, nothing is lost, apart from the time and effort to distill off, dry and redistill the acetone.

blue.magic said:
Yes I failed several projects: 3 kilos of mushroom substrate have rotten, I lost half of harmalas after purification mistake, then I lost gram of DMT by accidentaly spilling naphtha beaker, and then this...
It is only a failure if you learned nothing from the experience.

blue.magic said:
I don't want to try other methods. I want to know why this one does not work while it should and what am I doing wrong. Otherwise I will never understand some hidden mistake that is not mentioned anywhere.
It may take some careful investigation to pin down the causes. This could also involve time, study, effort and money. If you consider these an investment in a valuable course of practical learning (or perhaps even amusement), then you might end up with a sense of satisfaction. This should be all the pay-off that you should be interested in. What you mentioned in one of your more recent posts in this thread borders on sales and distribution. Don't do that here.
 
pitubo said:
How sure are you that your "acetone" is really acetone?

It's from chemical supplier and it's marked reagent grade.

pitubo said:
TEKs in the wiki are generally presumed to work and if they don't, there would have been a flurry of complaints.

I have a theory there is always some 100 mg loss from the process and some - say - 10% loss as the source material is not entirely pure.

This would explain why 300 mg of material resulted in 170 mg of product. While if most people convert 1 000+ mg, they don't experience such losses (the constant 100 mg loss is not that significant as the amount of source material increases).

However, since most people probably don't do small amounts, they would never notice and there wouldn't be complaints about the tek not giving near 100% recovery as it proposes.

pitubo said:
Since you appear to be in possession of a still, nothing is lost, apart from the time and effort to distill off, dry and redistill the acetone.

Yes distillation itself is a learning process and I can never get the temperature right. It's either too high or too low and it requires to sit there for hours and fiddle with the heating control.

All I needed was to remove water which at 69-70 C should be fine...

pitubo said:
It may take some careful investigation to pin down the causes. This could also involve time, study, effort and money. If you consider these an investment in a valuable course of practical learning (or perhaps even amusement), then you might end up with a sense of satisfaction. This should be all the pay-off that you should be interested in.

I already invested so much time and money it is no longer entertaining. It became a hard work so I at least wanted some kind, any kind of appreciation so I can keep motivated to continue...

As for the dontaions, benzyme has XMR link in the description so I thought it is okay. I woulnd't add it to my description otherwise.

I am at the verge of giving up since even the simplest tasks like converting DMT to fumarate seems to require elaborate lab skills reserved only to experienced chemists and people who were taught by them.
 
Nereus said:
Word of advice: don't look at these things to simply "pay you off in the future"

Well everything you do has to be rewarding in some way. Why would you do it otherwise then?

I think I have just too many projects apart from DMT extraction and it's already overwhelming. Each project requires a set skills and learning curve and since I am still newbie in most of them it appears I am a total failure...

Since I failed one project I tried others to get some satisfaction and then I failed other three and here I am...

Nereus said:
Sure, taking a couple of chem courses can be practical overall, but it's not like alotta people with 0 chem backround haven't succeeded to integrate the informations here and get satisfying results in the past. On the contrary, you'll find more self thought chemists here than academic ones, and I bet many learned a lot while being here.

No I have a feeling that "kichten chemists" with zero background and way more successful then me who did the study and bought couple of books and papers. I feel like people are more successful and are more talented.

Maybe it's not true, but I don't know. It just looks like doing the teks is effortless for most people. They often report 2.2% yield here and 1.7% yield there while they are clearly newbies... and me after 2 years is still not able to get over 1%...
 
blue.magic said:
Nereus said:
Word of advice: don't look at these things to simply "pay you off in the future"

Well everything you do has to be rewarding in some way. Why would you do it otherwise then?

:? Okay wow so stop science then because lots of research ends into nothing
 
Ulim said:
blue.magic said:
Nereus said:
Word of advice: don't look at these things to simply "pay you off in the future"

Well everything you do has to be rewarding in some way. Why would you do it otherwise then?

:? Okay wow so stop science then because lots of research ends into nothing

Most experiments begin as fun, then after two days or so it becomes pretty hard work.

Respect and appreciation is also kind of reward apart form the actual results obtained. But maybe the problem is I am sorrounded by people who either don't understand it or laugh at me when see me doing some chem stuff or don't know (thus appearing like weirdo to them) since I has to be moderately secretive about it.
 
blue.magic I am not going to comment further on your motivational lamentations, but I want to reemphasize my earlier questions about the nature of your acetone, that you did not respond to. A boiling point of more than 56 degrees hints at serious problems.

My own experience with distilling acetone - even without a fractionating column - is that dried acetone distills cleanly at 56 degrees. I never had to tweak the heating of the boiling flask, apart from making sure that the contents start boiling gently. After that, the set heating power drives the remainder of the distillation until the vapor temperature at the still head rises to 57 degrees.

Any structural deviation from the known boiling point should be taken as a matter of concern.

pitubo said:
blue.magic said:
I have distilled the acetone TWICE (with a fractional column - the vapor temp never exceeded 70 C and no, acetone does not form an azeotrope with water) and dried by excess MgSO4 which itself has just been oven dried for 2 hours on 250 C (which is excess by some standards).
Pure acetone boils at 56 degrees centigrade (Celsius). If you distill acetone, over a fractionating column even, and you collect any distillate that comes over at a temperature higher than that, you're not doing it right.

How sure are you that your "acetone" is really acetone? Suppliers do make mistakes occasionally. Methanol, various mixtures of methanol, ethanol, ethyl acetate and acetone could distill below 70 degrees and might cause the partial precipitation that you got.

I have done this procedure myself a few times using dried and distilled technical (hardware store) acetone and I mostly got nice needles after a night in the fridge. The only time when the result was powdery was when I used a mixture of dmt and nmt from an acacia extract.
 
pitubo said:
blue.magic I am not going to comment further on your motivational lamentations, but I want to reemphasize my earlier questions about the nature of your acetone, that you did not respond to. A boiling point of more than 56 degrees hints at serious problems.

Sorry I was mistaken, the temp was around 58 degrees centigrade, not 68. The vapor temperature never exceeded 59 degrees even by the end of distillation.

Please note the acetone has not been in contact with anything except dry plant material and air moisture. The distillate was single layer and crystal clear.

I was looking if there is any test for moisture content, like there is with ethanol (adding magnesium and observing if there is a reaction) but haven't found anything.

I can try evaporation test to see if there is any residual moisture but I highly doubt it. I have oven dried even the distillation apparatus and acetone has been transferred to (pre-dried) bottle right after distillation.

Also please note the product loss happened also with freshly opened bottle of acetone, which is reagent grade and guaranteed water content below 0.5%.
 
Oven drying the glassware is not necessary unless you are making grignard reagents or similar stuff that would be poisoned by minute amounts of water.

Perhaps you can do a crude test for water contents by adding a pinch of anhydrous copper sulphate to a sample of your acetone. It should go from white to blue or a blueish tinge if there is substantial water present.

Another consideration is to not go overboard with the acetone. Use only as much as is needed to dissolve the dmt and the stoichometric amount of fumaric acid. Add the FASA dropwise to the acetone/dmt with good stirring. Cover the mixing flask and let it stand for an hour and then put it in the fridge or freezer for a few hours.
 
pitubo said:
Oven drying the glassware is not necessary unless you are making grignard reagents or similar stuff that would be poisoned by minute amounts of water.

Perhaps you can do a crude test for water contents by adding a pinch of anhydrous copper sulphate to a sample of your acetone. It should go from white to blue or a blueish tinge if there is substantial water present.

Another consideration is to not go overboard with the acetone. Use only as much as is needed to dissolve the dmt and the stoichometric amount of fumaric acid. Add the FASA dropwise to the acetone/dmt with good stirring. Cover the mixing flask and let it stand for an hour and then put it in the fridge or freezer for a few hours.

Okay.

At first I followed the recipe from "SWIM's Psychedelic Cookbook". It advised to use 20 ml acetone to dissolve 1 gram DMT and 20 ml to dissolve 300 mg fumaric a. Then mix the two.

This recipe didn't work and then I found on wiki only a minimum amount of acetone should be used to dissolve the DMT like you wrote.

My DMT (300 mg) dissolved in just about 1 ml of acetone (a droplet basically) but there were tiny particles floating in it so I added few milliliters more - the particles haven't disappeared so I concluded these are some insolubles, not DMT. I used tall 50 ml beaker but a test tube or vial would be more appropriate...

I made FASA with excess fumaric a. and took the liquid with eyedropper.

I added FASA dropwise, always waited for clouds to settle and only added FASA to the clear supernatant liquid until no clouding occured.

The I decanted the solution and washed several times with fresh acetone.

I don't know if that's normal but dissolving the fumaric acid took very long time and lots of mixing. It has not dissolved readily but it needed lots of agitation. But the amount dissolved corresponds to the numbers I found on the web.

Next time I will use ice cold acetone and maybe two solvents. Maybe cold MEK would be better for washing as there is opportunity to remove impurities insoluble in just acetone.

Maybe dissolving DMT in NPS would also work better than with just acetone.

...however using just acetone is more straightforward and simple. I don't want to overcomplicate it.
 
More importantly:

Next time, save everything, dont throw anything away. Considering things dont just dissapear out of thin air, nothing is lost until you discard whatever portion has your DMT.
 
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