Disappointing yield using Q21Q21's TEK - ideas?

[VoidTraveler]

I've done an A/B TEK this weekend using Q21Q21's A/B TEK with vinegar and lime and had a very disappointing yield. Looking at it, I don't think I've even managed to get a 0.1 or 0.2% yield.

First of all: the materials that I've used are of the right chemical composition. I've gone to great lengths to acquire laboratory grade lime and the vinegar that I used contains 8% acetic acid. The naphtha that I used worked fine in a previous STB TEK. My MHRB was bought from mimosahostilis.mx and is a renowned source on these forums.

I have whole MHRB, so I used a coffee mill to chop them up in fibers and small quantities of powder. I made sure the fibers were are fine as possible and I measured off 100 grams of MHRB to get the hang of this TEK before trying a larger batch. When mixing in the vinegar I quickly noticed that the 100ml that I was supposed to use wasn't enough. So I added about 175ml of vinegar and approx the same amount of water. Thoroughly mixed it all and I let that mix sit for about an hour while I mixed it 4 to 5 times at various intervals. I weighed off the amount of lime that I was supposed to use and gradually mixed it in, concluded it was way too wet and kept adding lime. Now, I'm not entirely sure but I don't think I've added a factor 1.75 of the required lime to compensated for the higher amounts of water/vinegar. So, this could be a reason why the yield is so low.

Next up I let that mix sit for about 12 hours and at various intervals mixed it a bit. The day after I added the naphtha but used more than in the TEK, about 1.5x / 1.75x of what the TEK said. Again, I could've used too much and the DMT wouldn't crystallize due too much naphtha. So I'm currently evap'ing the naphtha in front of a fan.

So, there are a few things that I'm considering:
- Add more lime to the mix, stir it thoroughly, let it sit for 12 to 24 hours and then do another pull
- Evap half the naphtha and then do a freeze precip(currently happening)

Any other thoughts? Is there anything I can do with the current batch or should I consider it lost?

 

[ntwhtyouknw]

Be patient and try pulling once a day for a week.

 

[ntwhtyouknw]

See what your yield is after a week. Personally I'd even do another pull in two weeks from start.

 

[ntwhtyouknw]

Definitely DO NOT throw away. Everything sounds normal. Just be patient it will turn out fine.

 

[tele]

Sounds like you're doing everything right... Try adding hotter water bath when the naphtha is in. You can also pre heat the naphtha in hot water in a shot glass for example. More lime isn't a problem, so isn't the tek. Don't throw it away... Make sure to stir the naphtha around so it contacts all the mixture surface. I would recommend crumbly texture, less naphtha loss.
I had issues with low yield using self powdered bark, about 0,4%, the problem was solved with pre-powdered adenium bark.
If nothing else will work even for future mixtures, the problem is most likely with the MHRB.

 

[VoidTraveler]

Sounds like you're doing everything right... Try adding hotter water bath when the naphtha is in. You can also pre heat the naphtha in hot water in a shot glass for example. More lime isn't a problem, so isn't the tek. Don't throw it away... Make sure to stir the naphtha around so it contacts all the mixture surface. I would recommend crumbly texture, less naphtha loss.
I had issues with low yield using self powdered bark, about 0,4%, the problem was solved with pre-powdered adenium bark.
If nothing else will work even for future mixtures, the problem is most likely with the MHRB.

I used a thermometer after I added the naphtha to check the temp and extracted the naphtha at around 60 degrees Celsius. It could be a mixing problem and that I just didn't mix thoroughly enough. I'll do a pull tonight with a lower amount of naphtha and more mixing.

I'll also run a Lazyman's STB extraction later this week to see if it's a problem with the MHRB or with my use of the TEK.

 

[tele]

Sounds like you're doing everything right... Try adding hotter water bath when the naphtha is in. You can also pre heat the naphtha in hot water in a shot glass for example. More lime isn't a problem, so isn't the tek. Don't throw it away... Make sure to stir the naphtha around so it contacts all the mixture surface. I would recommend crumbly texture, less naphtha loss.
I had issues with low yield using self powdered bark, about 0,4%, the problem was solved with pre-powdered adenium bark.
If nothing else will work even for future mixtures, the problem is most likely with the MHRB.

I used a thermometer after I added the naphtha to check the temp and extracted the naphtha at around 60 degrees Celsius. It could be a mixing problem and that I just didn't mix thoroughly enough. I'll do a pull tonight with a lower amount of naphtha and more mixing.

I'll also run a Lazyman's STB extraction later this week to see if it's a problem with the MHRB or with my use of the TEK.

Try crumbly consistency and use about 1,5-2ml naphtha per 1g bark. Stir constantly for about 5 minutes and then pour off the naphtha, should work.

 

[VoidTraveler]

Try crumbly consistency and use about 1,5-2ml naphtha per 1g bark. Stir constantly for about 5 minutes and then pour off the naphtha, should work.

I'll try that. I'm not too concerned about losing naphtha because it's readily available and cheap. Of course, reducing the loss to a minimum is both economic and better for the environment. It's currently pea soup thick, so I'll put it on low(70 or 80 degrees Celsius) in the oven for half an hour. EDIT: Putting it in the oven for half an hour to save a little bit of naphtha doesn't sound very economic either. Nor environmentally saving.

As for my first two pulls: Over the course of the past few days I evaporated about 35% of the naphtha off and put it back in the freezer. I checked this morning and was somewhat disappointed with the amount that precipitated on my dish as it seemed even less now. Then I noticed that my fridge wasn't on it's coldest setting. So I changed it and currently I see a much larger yield than before the evap. Put it in the fridge last night and upped the temp this morning so I'll think I'll run it through a filter and put it to dry at around 8 tonight and then immediately do another pull. If I have to guess, I think I'll get about 300 to 500mg from my dish at this point. And tonight's pull should be a rather large pull then because the bark has been soaking for quite a while now.

 

[tele]

Try crumbly consistency and use about 1,5-2ml naphtha per 1g bark. Stir constantly for about 5 minutes and then pour off the naphtha, should work.

I'll try that. I'm not too concerned about losing naphtha because it's readily available and cheap. Of course, reducing the loss to a minimum is both economic and better for the environment. It's currently pea soup thick, so I'll put it on low(70 or 80 degrees Celsius) in the oven for half an hour. EDIT: Putting it in the oven for half an hour to save a little bit of naphtha doesn't sound very economic either. Nor environmentally saving.

As for my first two pulls: Over the course of the past few days I evaporated about 35% of the naphtha off and put it back in the freezer. I checked this morning and was somewhat disappointed with the amount that precipitated on my dish as it seemed even less now. Then I noticed that my fridge wasn't on it's coldest setting. So I changed it and currently I see a much larger yield than before the evap. Put it in the fridge last night and upped the temp this morning so I'll think I'll run it through a filter and put it to dry at around 8 tonight and then immediately do another pull. If I have to guess, I think I'll get about 300 to 500mg from my dish at this point. And tonight's pull should be a rather large pull then because the bark has been soaking for quite a while now.

Are you putting it in the fridge? Or did you actually mean freezer? Freezer is the way to go... If you used fridge, that's your problem with yield.

You can also dry it to crumbly by putting it under a fan. The point is, it doesn't have to be soupy.

No need to pre-evaporate with this tek. I have tested and there is very little difference.

 

[VoidTraveler]

Are you putting it in the fridge? Or did you actually mean freezer? Freezer is the way to go... If you used fridge, that's your problem with yield.

Language barrier. I'm actually putting it in the freezer, although I have a combination fridge/freezer. When I first pre-cipped it, my freezer was on it's coldest setting. And it is now again.

You can also dry it to crumbly by putting it under a fan. The point is, it doesn't have to be soupy.

I was planning on just ovening it. It's the quickest route.

No need to pre-evaporate with this tek. I have tested and there is very little difference.

That's what I thought. I think my initial low yield was due to a combination using too much naphtha and not enough mixing/contact with the MHRB mix during the pull. I just tossed the naphtha in, heated it till it got to 60C and did a little bit of mixing. During my Lazyman's STB I actually stirred vigorously to ensure a high yield. During tonight's pull I'll make sure to stir enough and I bet that'll saturate the naphtha enough to freeze precipitate it properly.

Thanks for the help and I'll report back when I have a dry batch with a yield.

 

[tele]

when you dry it make sure it's not bone dry but slightly moist, so it's crumbly. The finer the crumbles, the better.

 

[VoidTraveler]

My precipitation from yesterday is dry. It was a disappointing 110mg but it's pretty potent. I vaped about 20mgs and had a REALLY intense experience but no breakthrough yet.

I dried the mixture a bit more yesterday and then tipped in warm naphtha, heated it all up to 60C and thoroughly mixed(kept mixing it for 10 minutes while the naphtha heated to 60C). The naphtha that I pulled from the mix was a lot more yellowish than the first two pulls. However, stuck it in the freezer last night around 23:00 / 0:00 and this morning only a few tiny crystals formed, but the naphtha was very clouded. So kept it in the freezer in the hope that this pull will be a proper one. I'm going to do an STB on 200 or 300 grams on friday to see if the MHRB is low potentency and if it's not, I'm going to arrange some pH papers to see if it's a pH level issue.

 

[tele]

My precipitation from yesterday is dry. It was a disappointing 110mg but it's pretty potent. I vaped about 20mgs and had a REALLY intense experience but no breakthrough yet.

I dried the mixture a bit more yesterday and then tipped in warm naphtha, heated it all up to 60C and thoroughly mixed(kept mixing it for 10 minutes while the naphtha heated to 60C). The naphtha that I pulled from the mix was a lot more yellowish than the first two pulls. However, stuck it in the freezer last night around 23:00 / 0:00 and this morning only a few tiny crystals formed, but the naphtha was very clouded. So kept it in the freezer in the hope that this pull will be a proper one. I'm going to do an STB on 200 or 300 grams on friday to see if the MHRB is low potentency and if it's not, I'm going to arrange some pH papers to see if it's a pH level issue.

If it's clouded it means at least that there's DMT in it. Do not remove from the freeza before it's clear naphtha.

Usually after 24 hours the full yield is visible, but it's best to keep it for at least 48 hours.

PH testers is a good idea.
I really wonder why the yield is so low... Could be bark problem so let us know how the STB goes. good luck

 

[VoidTraveler]

Usually after 24 hours the full yield is visible, but it's best to keep it for at least 48 hours.

The current yield in the dish is disappointingly low. It wouldn't surprise me if it's not even enough for a single hit. I'm both annoyed and confused so I've just finished a HDPE jug and I'm going to do an STB with it tonight with 200 or 300 grams of powder. I'll probably do the pulls on sunday so that'll let the mix mature for a bit.

To make 100% sure it's not a pH problem I added extra lime to the mix as I won't be able to purchase pH testing papers until after the weekend. Added the lime, will mix more often and attempt another pull in 4 hours to see if it did any good. Of course, if it was a pH problem I'll probably be better off waiting till tomorrow night before doing a pull.

PH testers is a good idea.
I really wonder why the yield is so low... Could be bark problem so let us know how the STB goes. good luck

The bark is coming from Don Jose and I've read a lot of good stories about the quality of his bark. So I'm assuming that I'm doing something wrong. I'll report back later if I know more.

 

[Simon Jester]

Don't throw your MHBR mash away until you've fully pulled it and it doesn't smell even a little like indole alkaloids!!! There's still DMT in there otherwise!

I see two things that might result in a low yield in my experience:

Your acid stage is rather short... Yes, I realize it's longer than the tek suggests, but I find that four hours in 5% vinegar (no extra water) over low heat in a crock pot works best... any less time or less acid doesn't seem to properly acidify the MHRB. There's a difference in color and consistency that makes it easy to tell when the acid stage is done, once you get the hang of it.
---

Using more naptha per pull actually does not pull any more DMT than a minimal amount of naptha. The basics are that the amount of DMT you get from each pull is dependent on the concentration of DMT in the mash, whether it is totally basified (ph12), and how warm your naptha is... NOT how much naptha you use. Use only enough naptha per pull to allow the naptha to cover the surface of the MHRB mash while you are stirring it around. Also, try not to let the naptha get trapped in bubbles in the mash or it will soak in... just gently move the MHRB around under the thin layer of naptha, allowing all the MHRB to come in contact with the naptha.

You got a lot of naptha with a very low concentration of DMT. Try doing smaller pulls at a higher temp (150F usually gives me good results, and is safe so long as you do it in a crockpot or hot water bath, not on a stove). You will have less naptha, but it will be highly saturated with DMT (even yellowed). As you approach the end of the extraction, you will begin to pull a lot of yellow oils; At this time it is usually appropriate to lower the temp and use a bit more naptha to keep the oils at bay (though the oils are wonderfully psychoactive if you take the time to extract and separate them).

Letting it sit out to dry, grinding it up and pulling again is often pretty effective... I usually add a little bit of water and lime to keep the ph up and make it wet enough to dislike absorbing any solvent.

The better your pulls are, the more yellowed your DMT will be in the end. Simply toss it all in a clean precipitation jar, and then add just enough hot clean naptha to fully dissolve your crystals. Freeze precipitate and collect as before, and you'll have sparkly white freebase.

When you freeze precip, you should notice that the naptha becomes very cloudy after just a few hours in the freezer. This cloudiness is DMT that can no longer be held by the now more dense naptha, and falls out of the solution into suspension. This cloudy DMT will bind together like snowflakes and fall to the bottom of the container, and the cycle continues. After a couple of days, your crystals should be fully-formed and your naptha should be clear (though maybe yellow, it should not be cloudy. Cloudiness means there's more DMT in there that has yet to fall out)

You can recover the un-precipitated DMT and the yellow oils from your naptha by using this method, which will leave you with an extra (very potent) surprise and fresh clean naptha that can be reused.

Good Luck!

 

[tele]

Your acid stage is rather short... Yes, I realize it's longer than the tek suggests, but I find that four hours in 5% vinegar (no extra water) over low heat in a crock pot works best... any less time or less acid doesn't seem to properly acidify the MHRB. There's a difference in color and consistency that makes it easy to tell when the acid stage is done, once you get the hang of it.
--

But still, even if the acid step would be totally removed from the tek, it will be a STB tek which requires about 2-3 days to pull out anything significant.

But I would also recommend at least 2 hour acid step, just to be sure it's done properly. 5-10% vinegar is fine.

Quote from the q21 tek:
Note 2: If you were to choose not the acidification step, thus doing a STB lime tek, it would work... but would take periodic stirring over a minimum of 2 days before a significant yield will be achieve and several days more for the rest

The vinegar step is essential for the swiftness of the tek to be utilized.

 

[VoidTraveler]

Wow, that's a lot of solid advice you have there man! Thanks, I can work with that and I'll work that into my next attempt. The longer my naphtha is in the freeze, the bigger the crystals. I think I've removed it too quickly.

I'll use less naphtha next time. I'll tip in 50ml for the next pull. Also, I've made an STB bottle with 250grams of MHRB in 1.5l of waters. I tipped in 125ml of naphtha, you reckon that's too much? What factors do you use on mhrb:naphtha ratio?

 

[tele]

Wow, that's a lot of solid advice you have there man! Thanks, I can work with that and I'll work that into my next attempt. The longer my naphtha is in the freeze, the bigger the crystals. I think I've removed it too quickly.

I'll use less naphtha next time. I'll tip in 50ml for the next pull. Also, I've made an STB bottle with 250grams of MHRB in 1.5l of waters. I tipped in 125ml of naphtha, you reckon that's too much? What factors do you use on mhrb:naphtha ratio?

0,7ml-1,5ml is fine for 1g of MHRB. You don't need any less or more for better results. 1g bark and 1g solvent works well.

 

[VoidTraveler]

0,7ml-1,5ml is fine for 1g of MHRB. You don't need any less or more for better results. 1g bark and 1g solvent works well.

Well, it's been determined, I've done something wrong with the A/B. I've pulled my naphtha from my MHRB mix and put it in the freezer and I'm already seeing large quantities of tiny specs form in the bottom of the dish. That determines that the rootbark isn't of low quality. Of course, we still have to verify the end result and this was only my first pull. But from what I can see, a lot of yellow gooey. Definitely going to have to do a re-crystallization on this.

If this doesn't work out all the way I expected, I'll be getting myself some pH papers after the weekend and start from scratch with the newly gathered information.

 

[tele]

0,7ml-1,5ml is fine for 1g of MHRB. You don't need any less or more for better results. 1g bark and 1g solvent works well.

Well, it's been determined, I've done something wrong with the A/B. I've pulled my naphtha from my MHRB mix and put it in the freezer and I'm already seeing large quantities of tiny specs form in the bottom of the dish. That determines that the rootbark isn't of low quality. Of course, we still have to verify the end result and this was only my first pull. But from what I can see, a lot of yellow gooey. Definitely going to have to do a re-crystallization on this.

If this doesn't work out all the way I expected, I'll be getting myself some pH papers after the weekend and start from scratch with the newly gathered information.

I never get any large amounts of yellow goo with q21's tek. Sometimes there are spots or specks or yellow oil, which is easily just scraped off. However, it does have it's own effect on the spice and it's kind of nice. Let us know if you find out what was the problem.