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Low yield

Crilas31

Crilas31

Rising Star
Used a STB tek on 100g of MHRB
750ml of distilled water
100g of sodium hydroxide (I know it’s a lot I didn’t have ph strips so I overused to make sure I met ph requirements)
150ml of Vm&p Naphtha (clean evap test)
Just harvested from my Pyrex of the first pull on my first attempt at doing this and only yielded roughly 200mg. My question is this a normal yield amount for one pull? Or did I go wrong somewhere, bark quality not good etc… if you have any further questions of my method I’d love to answer. Sorry kind of a newbie to this whole thing
 
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Crilas31 said:
Used a STB tek on 100g of MHRB
750ml of distilled water
100g of sodium hydroxide (I know it’s a lot I didn’t have ph strips so I overused to make sure I met ph requirements)
150ml of Vm&p Naphtha (clean evap test)
Just harvested from my Pyrex of the first pull on my first attempt at doing this and only yielded roughly 200mg. My question is this a normal yield amount for one pull? Or did I go wrong somewhere, bark quality not good etc… if you have any further questions of my method I’d love to answer. Sorry kind of a newbie to this whole thing
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Worthy to note I did water wash twice before starting freeze process with warm distilled water.
 
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I think 1% yield is average, so on 100g of bark, you might expect 1g.

Solubility of DMT in naphtha is 2.93 g in 100 ml at room temp. So you could theoretically pull all your DMT in one pull.

I don't do STB teks so idk what normal is, but I'm guessing it takes time for the lye to break down the bark. Could try heating the jar up on the next pull.

You also want to make sure there's a pinch of base in your distilled wash water. Otherwise it can absorb CO2 and turn slightly acidic, which could remove some freebase molecules in the wash.
 
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Sometimes you'll get better yields, sometimes you'll get lower yields. There is nothing inherently wrong about getting 0,2% in the first pull, its on the lower side but its something at least.

but I'm guessing it takes time for the lye to break down the bark. Could try heating the jar up on the next pull.
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This is correct. If you do the first pull on a STB inmediatly, there is no time for the base to destroy plant cell walls. Both time and heat aid with that.

A second pull might still result in a higher yield.

There is no need for heat, and I don't personally use it until the last pull, but heat does help to extract a little more.

I think 1% yield is average
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This is also correct. That's the average, but I've sometimes gotten as low as 0.5% total, and as high as 2.3% total. A friend of mine once got 0.1% total, it was a bit devastating... but it is what it is.

Rootbark quality matters. The TEK matters. Your ability to perform it matters.

Just keep trying ;)
 
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Crilas31 said:
Think it would be safe to just basify some more distilled water and just pour it in? I mean I’m on my 3rd pull (I’m assuming my last) of this bark so not sure how much help it would be now but still for future reference the question still stands. Thank you all for your fast replies, will take this all in consideration.
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Yes, this would be fine and very likely rather helpful in improving yields. You may need to do a fourth and fifth - or even more pulls in total if you're still getting results from the fifth one, considering you've had poor yields from the first couple of pulls.
 
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pantostao said:
Sometimes you'll get better yields, sometimes you'll get lower yields. There is nothing inherently wrong about getting 0,2% in the first pull, its on the lower side but its something at least.



This is correct. If you do the first pull on a STB inmediatly, there is no time for the base to destroy plant cell walls. Both time and heat aid with that.

A second pull might still result in a higher yield.

There is no need for heat, and I don't personally use it until the last pull, but heat does help to extract a little more.



This is also correct. That's the average, but I've sometimes gotten as low as 0.5% total, and as high as 2.3% total. A friend of mine once got 0.1% total, it was a bit devastating... but it is what it is.

Rootbark quality matters. The TEK matters. Your ability to perform it matters.

Just keep trying ;)
Click to expand...
I tried letting everything settle each time I mixed the lye water with the bark. I honestly think I was waiting a little too long between stirs. I stirred it about 8 times with vigorous swirling, no inverting or shaking. With about 2-4 hours in between each stir. Is this an efficient time interval of letting it sit and settle? Also worthy to note I allowed the lye water to sit over night to come to room temp before I mixed it with my bark. All in all it was my first time doing this extraction so happy to see any sort of harvest but still would love to fine tune it as I go! Thank you for the good observations, much appreciation
 
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Crilas31 said:
I tried letting everything settle each time I mixed the lye water with the bark. I honestly think I was waiting a little too long between stirs. I stirred it about 8 times with vigorous swirling, no inverting or shaking. With about 2-4 hours in between each stir. Is this an efficient time interval of letting it sit and settle? Also worthy to note I allowed the lye water to sit over night to come to room temp before I mixed it with my bark. All in all it was my first time doing this extraction so happy to see any sort of harvest but still would love to fine tune it as I go! Thank you for the good observations, much appreciation
Click to expand...
If anything, that's an unnecessarily long settling time. Migration of the freebase from the aqueous phase into the naphtha occurs at the phase interface, so you'd be better of stirring for longer and only leaving things to settle for as long as it takes to separate back into two distinct phases. Stirring maximises the contact surface area between the two phases, which is where the extraction proper takes place.

You only really need to concern yourself about a complete separation on the very last pull, and there are various ways of preventing droplets of base soup from getting into your crystallisation dish (such as the water washes that you did). And I'd hope that maybe you kept that washing water, since you could return it to the base soup as a convenient way of adding extra water while avoiding losses.

Cooling the lye water overnight shouldn't present any special problems if it was kept in a reasonably well-sealed and lye-resistant container.
 
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Crilas31 said:
Think it would be safe to just basify some more distilled water and just pour it in? I mean I’m on my 3rd pull (I’m assuming my last) of this bark so not sure how much help it would be now but still for future reference the question still stands. Thank you all for your fast replies, will take this all in consideration.
Click to expand...
Yes I would just add water since you already added 100g lye.

Crilas31 said:
I tried letting everything settle each time I mixed the lye water with the bark. I honestly think I was waiting a little too long between stirs. I stirred it about 8 times with vigorous swirling, no inverting or shaking. With about 2-4 hours in between each stir. Is this an efficient time interval of letting it sit and settle? Also worthy to note I allowed the lye water to sit over night to come to room temp before I mixed it with my bark. All in all it was my first time doing this extraction so happy to see any sort of harvest but still would love to fine tune it as I go! Thank you for the good observations, much appreciation
Click to expand...
You mean 8 stirs with 2-4 hours in between for each pull? That's overkill, you can stir 3-4 times with 15 mins in between and then let it sit longer after the last stir to ensure good seperation before the pull. And during the swirling do you see the NPS layer disapearing into the base soup before seperating again? Maybe also turn it on its side to increase the contact surface and give it some gentle shaking.
 
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Transform said:
If anything, that's an unnecessarily long settling time. Migration of the freebase from the aqueous phase into the naphtha occurs at the phase interface, so you'd be better of stirring for longer and only leaving things to settle for as long as it takes to separate back into two distinct phases. Stirring maximises the contact surface area between the two phases, which is where the extraction proper takes place.

You only really need to concern yourself about a complete separation on the very last pull, and there are various ways of preventing droplets of base soup from getting into your crystallisation dish (such as the water washes that you did). And I'd hope that maybe you kept that washing water, since you could return it to the base soup as a convenient way of adding extra water while avoiding losses.

Cooling the lye water overnight shouldn't present any special problems if it was kept in a reasonably well-sealed and lye-resistant container.
Click to expand...
Got it okay.
Maybe I worded it weird but I meant before naphtha was added. The breaking down process of the bark I guess it would be. After naphtha was added I stirred about 4 times with about 45-an hour in between to allow for separation. I am having a problem with the solvent not separating as fast now though on my 3rd pull. I stirred and went to sleep last night and woke up to the solvent still not being separated so wondering if it’s gotten to cool where I store it.
Yes I did keep that water! I didn’t add it back though as I should after seeing your suggestions, I have it stored in a separate mason jar right now though that can be added back.
 
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Sakkadelic said:
Yes I would just add water since you already added 100g lye
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Sakkadelic said:
Yes I would just add water since you already added 100g lye.


You mean 8 stirs with 2-4 hours in between for each pull? That's overkill, you can stir 3-4 times with 15 mins in between and then let it sit longer after the last stir to ensure good seperation before the pull. And during the swirling do you see the NPS layer disapearing into the base soup before seperating again? Maybe also turn it on its side to increase the contact surface and give it some gentle shaking.
Click to expand...
Yes, but maybe I made it confusing The naphtha wasn’t in the equation at this point. When naphtha was present I did about 4 stirs with hour intervals to allow for separation.
Yes, I did see the solvent mixing in with the base soup to the point I could not see the separate layers. Got it, I’ll try that!
 
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Crilas31 said:
Got it okay.
Maybe I worded it weird but I meant before naphtha was added. The breaking down process of the bark I guess it would be. After naphtha was added I stirred about 4 times with about 45-an hour in between to allow for separation. I am having a problem with the solvent not separating as fast now though on my 3rd pull. I stirred and went to sleep last night and woke up to the solvent still not being separated so wondering if it’s gotten to cool where I store it.
Yes I did keep that water! I didn’t add it back though as I should after seeing your suggestions, I have it stored in a separate mason jar right now though that can be added back.
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Ah yes - I should have read a bit more carefully! I've never bothered to let the bark soak that long so this preconception made me blind to exactly what you'd written.

Dilution should help to free up some of your trapped naphtha. Maybe add a dash of base to your washing water before adding it back into the extraction mixture, too.
 
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