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Acacia confusa extraction ?? Options
 
highc
#1 Posted : 2/28/2015 8:52:28 AM
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If one were to use use joshisom's tek what would result if you evaporated all the solvent instead of freeze precipitate? Would it still yield similar results or would there be extra alkaloids that don't fall out from freezing?
 

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concombres
#2 Posted : 2/28/2015 9:40:07 AM

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highc wrote:
If one were to use use joshisom's tek what would result if you evaporated all the solvent instead of freeze precipitate? Would it still yield similar results or would there be extra alkaloids that don't fall out from freezing?


You can evaporate if you'd like. Freeze precipitation produces a cleaner product.

I'd maybe do a mini a/b & freeze precip first, then recrystallize in naphtha or heptane & let it evaporate slowly over the course of however long with no agitation or airflow blowing on it.

Should result in nice clean large crystals if you do it that way.
 
fathomlessness
#3 Posted : 2/28/2015 1:08:23 PM

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concombres wrote:
highc wrote:
If one were to use use joshisom's tek what would result if you evaporated all the solvent instead of freeze precipitate? Would it still yield similar results or would there be extra alkaloids that don't fall out from freezing?


You can evaporate if you'd like. Freeze precipitation produces a cleaner product.

I'd maybe do a mini a/b & freeze precip first, then recrystallize in naphtha or heptane & let it evaporate slowly over the course of however long with no agitation or airflow blowing on it.


Yep, or freeze precipitate the clean crystals then whats left (wax and goo) dissolve in acetone very easily and put it on some herb of your choice.
 
Tryptallmine
#4 Posted : 3/1/2015 1:14:38 AM

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If he takes the time to do the mini A/B on all his pulls he won't need to re-x unless he's got some base in there. I just finished up a Confusa extraction yesterday having not worked with it much before. It's far less fatty than A.Maidenii or A.Obtusifolia. More in line with MHRB I think.

What I've been doing is collecting all my pulls into a coffee peculator (looks like a tall beaker) and leaving it in a heat bath while I continue further pulls. After the 40 minutes or so that it takes you to pull your solvent, 97% of any base/contaminants sticks to the bottom of the peculator. As it's a lipped glass, it makes it incredibly easy to pour it off leaving behind the contaminants.

Put that cleaned up solvent into your mini A/B and the results are flawless after 18 hours in freeze precip.

 
concombres
#5 Posted : 3/1/2015 1:38:22 AM

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Tryptallmine wrote:
If he takes the time to do the mini A/B on all his pulls he won't need to re-x unless he's got some base in there. I just finished up a Confusa extraction yesterday having not worked with it much before. It's far less fatty than A.Maidenii or A.Obtusifolia. More in line with MHRB I think.

What I've been doing is collecting all my pulls into a coffee peculator (looks like a tall beaker) and leaving it in a heat bath while I continue further pulls. After the 40 minutes or so that it takes you to pull your solvent, 97% of any base/contaminants sticks to the bottom of the peculator. As it's a lipped glass, it makes it incredibly easy to pour it off leaving behind the contaminants.

Put that cleaned up solvent into your mini A/B and the results are flawless after 18 hours in freeze precip.



I say re-x because solvent always takes on some minute amount of water. Even with mini a/b it'll pick up a little basic water from the solution.

I'd reccommend washing the dry spice in cold distilled water with ph raised to 8-9 to remove any further basic contamination. But re-x should at the very least get rid of a good percentage of the already tiny amount of base left over in the product due to lye not being soluble in hydrocarbon solvents. It should stay trapped in the goo.

The spice after mini a/b is perfectly smokable, but i prefer to go the extra mile for higher purity.
Plus re-x gives nice glassy crystal shards when spice is already cleaned up nicely Thumbs up
 
Tryptallmine
#6 Posted : 3/1/2015 2:21:37 AM

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Aww cmon!

I'm pretty astounded, got 2.3g from 100g Confusa.

No you've got me thinking about doing a re-x. I do have another few grams from the last extraction I could throw together and re-x 5g to grow some reasonably big fat crystals?



 
concombres
#7 Posted : 3/1/2015 2:53:31 AM

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Tryptallmine wrote:
Aww cmon!

Do you really think it's worth re-x'ing this lot? If I could grow some pretty crystals I'd give it ago?

I'm pretty astounded, got 2.3g from 100g Confusa.





Picture isn't showing up.
If you got 2.3g from 100g acacia thats ~2.3%. There is most likely some nmt and/or oils left over.

Re-x should remove any of that left over, you should be left with even purer spice than what you already have (with mini a/b it's got to be pretty clean already though).

It will grow nice crystals but it can be tricky to get them bigger than 25-30mg worth.

I still can't seem to get the nice clear branching ones like this.
But i do get some nice clear ones starting.
Maybe re-x in a tall, thin container like a test tube cooled slowly & insulated then moved into the fridge for a week or so then freezer.


 
Tryptallmine
#8 Posted : 3/1/2015 2:58:23 AM

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Yeah, I'm not sure why they pictures didn't show. I think annihilating all of the exif data on the image stopped it from showing. Image metadata should still be clean.

I'll try again here. Didn't seem like any oil or goo at all. It always scrapes a completely dry product with the Mini A/B

The one spec of orange on the plate of spice is actually a breadcrumb
Tryptallmine attached the following image(s):
ex2.jpg (194kb) downloaded 150 time(s).
ex6.jpg (89kb) downloaded 149 time(s).
ex5.jpg (218kb) downloaded 145 time(s).
 
concombres
#9 Posted : 3/1/2015 3:05:16 AM

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Yeah that looks to be pretty clean Thumbs up

Did you weigh out exactly 100g?
I always end up with a little extra bark going in & it boosts yeilds a little. No use in pouring a few grams of bark back into the bag Laughing

I have had spice that was pretty white leave behind some boogery stuff on re-x after mini a/b but not much.

Looks like you have some very high quality acacia Big grin

You may very well be able to get some very nice crystals with 5g. I've only ever re-xed 1g at a time.
Next extraction i've been planning on doing 3 100g extracrions back to back combining yeilds & mini a/b then re-x all at once all in pursuit of crystals like the ones pictured Laughing
I Don't even want to think about how long it'll take me to burn through all that spice 25mg at a time.
 
Tryptallmine
#10 Posted : 3/1/2015 3:08:44 AM

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concombres wrote:
Yeah that looks to be pretty clean Thumbs up

Did you weigh out exactly 100g?
I always end up with a little extra bark going in & it boosts yeilds a little. No use in pouring a few grams of bark back into the bag Laughing

I have had spice that was pretty white leave behind some boogery stuff on re-x after mini a/b but not much.

Looks like you have some very high quality acacia Big grin


Yeah you're right, I did tip the rest of the bag in, wouldn't have been much more than ~3-5g.

I did put an extra 20g of NaOH in the 'top off water' when basing. I didn't feel like it had the right colour, maybe that had something to do with it.
 
concombres
#11 Posted : 3/1/2015 3:16:50 AM

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Tryptallmine wrote:
concombres wrote:
Yeah that looks to be pretty clean Thumbs up

Did you weigh out exactly 100g?
I always end up with a little extra bark going in & it boosts yeilds a little. No use in pouring a few grams of bark back into the bag Laughing

I have had spice that was pretty white leave behind some boogery stuff on re-x after mini a/b but not much.

Looks like you have some very high quality acacia Big grin


Yeah you're right, I did tip the rest of the bag in, wouldn't have been much more than ~3-5g.

I did put an extra 20g of NaOH in the 'top off water' when basing. I didn't feel like it had the right colour, maybe that had something to do with it.


That would add in about an extra 100mg or so at 2%.
I've occasionally seen others yeild a bit over 2% & it's happened to me once with mhrb.

I woudln't worry too much about it.
 
Tryptallmine
#12 Posted : 3/1/2015 3:50:25 AM

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concombres wrote:


You may very well be able to get some very nice crystals with 5g. I've only ever re-xed 1g at a time.
Next extraction i've been planning on doing 3 100g extracrions back to back combining yeilds & mini a/b then re-x all at once all in pursuit of crystals like the ones pictured Laughing
I Don't even want to think about how long it'll take me to burn through all that spice 25mg at a time.


Yeah that's it. I have no real use for 5g, it's enough for 10+ years.

About the only other fun to be had with it is trying to grow bad ass crystals.

I might re-x 4g today in as little volume of naphtha as I can and allow it to crystallize in a rack of test tubes. With near boiling naphtha I think you should be able to dissolve 4g in say 50ml or so. Maybe keep feeding a single test tube?
 
concombres
#13 Posted : 3/1/2015 4:57:32 AM

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Tryptallmine wrote:
concombres wrote:


You may very well be able to get some very nice crystals with 5g. I've only ever re-xed 1g at a time.
Next extraction i've been planning on doing 3 100g extracrions back to back combining yeilds & mini a/b then re-x all at once all in pursuit of crystals like the ones pictured Laughing
I Don't even want to think about how long it'll take me to burn through all that spice 25mg at a time.


Yeah that's it. I have no real use for 5g, it's enough for 10+ years.

About the only other fun to be had with it is trying to grow bad ass crystals.

I might re-x 4g today in as little volume of naphtha as I can and allow it to crystallize in a rack of test tubes. With near boiling naphtha I think you should be able to dissolve 4g in say 50ml or so. Maybe keep feeding a single test tube?


Usually what i do is have a container partially submerged in a crockpot on high so doesnt instantly cool the solvent. Once thats up to temperature drop your spice into a separate test tube, bring some naphtha up to 120°f & drip it in a few drops at a time until the spice all dissolves. It usually leaves a pile of goop. Once all that is left undissolved is goop i transfer the saturated solvent into the warm container in the heat bath.
Go back with 5-10ml more heated solvent 2x & try to get anything left over in the goop, then go back with another 3ml the last time & keep all the saturated naphtha in the warmed up container.
After ~45minutes i drop the crockpot to medium & let it stay there for a few hours until temp stabilizes & then drop to low. After low it goes off & once the water is cooled to room temp i leave it sit a few days.

I havn't tried test tubes yet but i've been meaning to. I don't know much about crystal formation but it seems like in a skinny container the crystals would have the tendency to group closer & connect to form a single cluster or a few very large ones.
Insulating & cooling allows for temperature to drop at a slow enough rate that crystals should continue growing rather than dropping out as powder like freeze precip normally does.

 
Tryptallmine
#14 Posted : 3/1/2015 9:42:22 PM

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I just finished re-x'ing 3.5g in a small 50ml beaker. It's been cooling for some hours now. The beaker was insulated with tissue paper inside a whiskey glass. That was further wrapped in a little bubble wrap then covered with an inverted 500ml pyrex jug. It's tucked away in the back of a draw now to slowly and hopefully grow a big crystal.

Took around 25-27ml of Naphtha to dissolve an 8 ball over subsequent additions of solvent.

I Left it for a while but nothing settled out, apart from a few tiny impurities which were visually identifiable in the freebase such as an eye lash and grain of dirt etc.

It kind of leads me to believe that leaving your mini A/B pulls in a heat bath for 40 odd minutes before decanting into a crystallizing dish effectively achieves the same result as a re-x. I mean it really is the same thing with just a lot more solvent. It'd explain why I'm pulling very clean product with all the extractions.

 
concombres
#15 Posted : 3/1/2015 11:15:09 PM

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Tryptallmine wrote:
I just finished re-x'ing 3.5g in a small 50ml beaker. It's been cooling for some hours now. The beaker was insulated with tissue paper inside a whiskey glass. That was further wrapped in a little bubble wrap then covered with an inverted 500ml pyrex jug. It's tucked away in the back of a draw now to slowly and hopefully grow a big crystal.

Took around 25-27ml of Naphtha to dissolve an 8 ball over subsequent additions of solvent.

I Left it for a while but nothing settled out, apart from a few tiny impurities which were visually identifiable in the freebase such as an eye lash and grain of dirt etc.

It kind of leads me to believe that leaving your mini A/B pulls in a heat bath for 40 odd minutes before decanting into a crystallizing dish effectively achieves the same result as a re-x. I mean it really is the same thing with just a lot more solvent. It'd explain why I'm pulling very clean product with all the extractions.



Yeah yout spice looked pretty clean from what i saw Thumbs up
The mini a/b does a good job at cleanup but i'm a bit paranoid & ocd about purity. I usually go overkill with cleanups.
Once temp drops enough for crystals to form post some pics Big grin

Maybe let the remaining solvent evap to continue crystal growth. I can't see it holding much back though considering you got a whole 3.5g into 25ml
 
Tryptallmine
#16 Posted : 3/1/2015 11:43:53 PM

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concombres wrote:
Tryptallmine wrote:
I just finished re-x'ing 3.5g in a small 50ml beaker. It's been cooling for some hours now. The beaker was insulated with tissue paper inside a whiskey glass. That was further wrapped in a little bubble wrap then covered with an inverted 500ml pyrex jug. It's tucked away in the back of a draw now to slowly and hopefully grow a big crystal.

Took around 25-27ml of Naphtha to dissolve an 8 ball over subsequent additions of solvent.

I Left it for a while but nothing settled out, apart from a few tiny impurities which were visually identifiable in the freebase such as an eye lash and grain of dirt etc.

It kind of leads me to believe that leaving your mini A/B pulls in a heat bath for 40 odd minutes before decanting into a crystallizing dish effectively achieves the same result as a re-x. I mean it really is the same thing with just a lot more solvent. It'd explain why I'm pulling very clean product with all the extractions.



Yeah yout spice looked pretty clean from what i saw Thumbs up
The mini a/b does a good job at cleanup but i'm a bit paranoid & ocd about purity. I usually go overkill with cleanups.
Once temp drops enough for crystals to form post some pics Big grin

Maybe let the remaining solvent evap to continue crystal growth. I can't see it holding much back though considering you got a whole 3.5g into 25ml


I'll put some pictures up later, the crystal formation doesn't look as cool as I'd hoped. I might redissolve it again with ~60-100ml of solvent so the temperature doesn't change so rapidly.

Once the temp dropped below a certain level it was like an explosion of crystals. One minute there was a few specs on the bottom of the beaker, 5 minutes later there was what looked to be 500-1000mg rocks all around.

I think the beaker is probably too small with not enough surface area for 3.5g. It'll be one clump of crystals, if I can even dry it. I might have been better off using a wider bottom glass such as the scotch glass.

I really should have started another thread, I have a habit of thread jacking.

 
Tryptallmine
#17 Posted : 3/2/2015 9:06:03 AM

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Ahh, I screwed it up. Started turning dirty with boring looking crystals so I just re-x'ed again and put it back in a dish for crystallizing normally under freeze precip conditions.

I'll just have to blaze it, one day at a time...
 
 
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