critique my plan

[wolf8312]

Hey I was planning on doing an AB extraction probably using the max iron technique. So I was hoping that you good folks could maybe have a read and point out any potential flaws in my plan....

I will and want to use the proper equipment for the job -such as Buchner and a separation funnel etc- as I want my starting material before adding the base/naphtha to be as clean and filtered as possible.

I have decided to proceed in much the same way as I would with Ayahuasca and do a three times extraction, filter it through a tee-shirt, and then run it through the Buchner funnel a couple of times. When it is clean I plan to boil this (3x) all down to about 500 mls maybe even less as I won’t be using more than 100 grams for my first time. This should still be plenty enough water right?

After this I'll add salt and increase ionization after which I'll proceed to add the base and naphtha respectively.

Recrystalization I was thining about just using naphtha but would Hexene perhaps be a better idea?

 

[concombres]

Yout method looks sound. You're basically just doing the acid boil phase of an a/b when you brew, so your right on track.

You want real clean liquid if your using a separatory funnel. A buchner funnel with filter will clog FAST even after a t-shirt filtration.
You should probably filter as much out as you can before reduction & let it settle in the fridge for 3+ days so all the sludge can sink & you can pippette off or decant most of the clean liquid & then run that thru the buchner filter.

You wont be able to get all the water away from the sludge cleanly, but more water can be added later & the sludge can settle again. After 2x you should get 99% of the dmt left in the water you couldn't decant away from the sludge cleanly.

500ml may not be enough water for 100g. You should ideally reduce until you notice the liquid thickening. If it gets too thick you can just add more water.
When it's really thick you end up with emulsions & trapped solvent.

The rest is about right & heptane is the best recrystallization solvent but naphtha will work as well.

 

[wolf8312]

Thanks dude then I'll follow your advice and make use of the fridge as well. My sep funnel is 1000 mls (also have a 500ml) accounting for the base and naphtha what would be an acceptable volume of water to boil the 3X down to then?

Think I'll just go with naphtha for re-X and -even though it's more expensive to get offline- will probably just get a couple of 100ml cans of Zippo.

As I am going to be using mimosa a defat wont be needed right?

 

[concombres]

Thanks dude then I'll follow your advice and make use of the fridge as well. My sep funnel is 1000 mls (also have a 500ml) accounting for the base and naphtha what would be an acceptable volume of water to boil the 3X down to then?

Think I'll just go with naphtha for re-X and -even though it's more expensive to get offline- will probably just get a couple of 100ml cans of Zippo.

As I am going to be using mimosa a defat wont be needed right?

You should be fine reducing to 500ml after the boils are combined, filtered, de-sludged, & ran through a buchner filter.
The liquid only gets thick during reduction if it's not very clean. It should not be a problem after all the filtering & settling.
100g only has at most 2g dmt so 500ml water can for sure hold that.

& yeah you dont need a defat for mimosa.

& man i would buy naphtha at home depot or lowes in cash. It's like $20 a gallon. If they question you, your painting.
Deffinately keep that off the same accounts & credit cards used to buy mimosa. Thats a big no-no. If big brother decides to get nosey for any reason your cc statement or paypal would be a dead give away. Don't make it that easy.
Same goes for lye. Don't buy it at the same store as the naphtha OR at the very least go back later & have someone else run in for you while you wait in the car.

 

[wolf8312]

Yeah thanks dude and dont worry my mimosa is still whole and has been in the freezer these past two years!

I have an international debit card but only for the occasional ethnobotanical here and there and I dont dump everything on that one card!

Thanks for all the help got a very clear idea now!

 

[1ce]

My büchner funnel has always worked real well? What's your vacuum source?

 

[concombres]

My büchner funnel has always worked real well? What's your vacuum source?

:lol: glad you caught that. I didnt see anything about a pump, Just the buchner funnel & i never thought twice. I'm half asleep riding the train home from work so my attention to detail & thought processes are a bit skewed.

 

[wolf8312]

My büchner funnel has always worked real well? What's your vacuum source?

I'm gonna use a small electric pump with a trapping glass. I was thinking of just getting a hand pump but they sold all the tubing together with the funnel and filter paper for a reasonable price so it saved messing about. Haven't tried it yet though!

 

[1ce]

A good teflon pump is expensive. So make sure to use s trap for your solvents or a water aspirator since you don't want to flood a convection motor with fumes.

Filtration will be extremely fast and simple. I use the same equipment, best of luck on your extraction!

 

[1ce]

Further notes: Yes, hexane works much better if you have it available. I usually filter after the acid boil and wash with naptna.

You aren't going to need the bark hanging around once the acid boil is done. Idk what equipment you use for the boil, but I boil it under reflux for 24 hours at 2-3ph. What do you plan on using?

 

[wolf8312]

Nothing fancy for the acid boil just planning to do it in much the same way as I make Ayahuasca on a stove. Thanks buddy!

 

[1ce]

Nothing fancy for the acid boil just planning to do it in much the same way as I make Ayahuasca on a stove. Thanks buddy!

I got ya, one real simple thing you can do that would function similarly to a reflux setup is perhaps a noodle calendar over your pot, with some icey brine water. Maybe have this in a bag. One of the determining factors of solubility of a solvent (this time it's water) is the amount used.

I don't know how much a 100ml loss would detriment this (probably hardly at all) but that's 1 kitchen alternative one could employ without boiling down their water too much.

 

[wolf8312]

I might look into that if I find the above method to be flawed. I reckon that 500 Mls should be fine as long as I get the filtering right. Might look into getting a reflux setup like yours in the future but as I went with Quartz for my own glassware and sep funnels etc I don't think I am gonna buy anything else for a while!

One question is distilled water better than just spring or even tap water?

 

[1ce]

Probably not with this extraction unless it was chlorinated. I stay away from tap water just to avoid residue on my glass and extra cleaning. Some processes are more critical. You wouldn't use anything but the cleanest water if working up LSD would you?

Unless it's chlorinated you're perfectly fine bro. Acetone cleans your glass real well. And a free brotip: loosen the nut and pull the stopcock out a bit, that way it won't get stuck next time you go to use it.

Here, it isn't much, generally for beginners who understand a bit of chem but I think you (and others) could benefit. http://s000.tinyupload.com/index.php?file_id=27483671353701115222

Organic chemistry survival manual.

 

[wolf8312]

Thanks bud currently just working my way through organic chemistry as a second language! I have been teaching myself from youtube and two other text books.

As a second language is wonderful cause it has so many practice problems but I am concerned that although I am fully committed and determined to learn OC (pretty much loving it and addicted now) I am not getting any lab experience. That's the main reason I am doing the extraction actually to get some lab work under my belt! Lab survival is exactly what I need so truly thanks a lot buddy!

 

[1ce]

Haha yeah, that's why I built my own lab it took ages but I've got my own clean room and everything. You got this dude, I think you'll find DMT extractions from bark to be too easy

Edit:

Something depressing happened today, I thought I'd tell you about it because it happens eventually. Cracks. I have to toss the damned thing out and it breaks my heart in doing so:

 

[wolf8312]

Oh dear!

What is the glass you are using there? Borosilicate?

One reason why I went with quartz was that I was told it can withstand much higher temperatures. Not really needed for anything except my erlenmeyer flasks I suppose (I even bouught a quartz funnel lol) but still you can be damned sure I am going to mother and protect all of my pieces!

Hopefully this in itself will contribute towards a more careful and conscientious approach to my work!

Am I being naive to suppose that a round bottom made from quartz would not end up cracking eventually as yours has there?

Still no matter my crystalline glassware is beautiful!

 

[1ce]

Haha yeah, freshly clean glass makes me smile. Just something about it. Yeah, borosilicate 1000ml round bottom flask. Nothing special about it. I was in a hurry and it was placed right onto a hotplate.

There's the heavy walled flasks and the quartz. Quartz I can see if you're boiling sulfuric acid (JUST AN EXAMPLE!) which has a rediculously high boiling temp. Even this piece here lasted me ages with gentle care. I picked up a case of these for $90 bucks a couple years back. =]

I don't reckon you'll be doing anything serious like that so a quartz flask will probably last until you drop it.