Cold pulls

[sbc1]

I'm just wondering whether it's best to pull cold/room temperature or heat the mixture or just heat the solvent I've always done a hot water bath and heated the bottle but I want to stop that as it's a pain.
I'm currently doing my first 2/3 pulls with N-hexane at room temperature then switching to naphtha.
Should I heat up the N-hexane or leave it, if I keep pulling with N-hexane or naphtha cold/room temp would I still pull everything but would need more pulls. Thanks

 

[Th Entity]

Hey sbc1
From my reading, some chemists suggest that only the solvent should be heated, and the basic AQ solution kept at room temperature, but after mixing the warm solvent with the roomtemp basic AQ solution temperature will equilibrate within seconds while mixing. But if you heat both basic AQ solution and solvent you will pull more plant fats/oils which we dont want. Most solutes dissolve better in warm/hot solvents, warmer solvent = more saturated pull.

 

[sbc1]

Hey sbc1
From my reading, some chemists suggest that only the solvent should be heated, and the basic AQ solution kept at room temperature, but after mixing the warm solvent with the roomtemp basic AQ solution temperature will equilibrate within seconds while mixing. But if you heat both basic AQ solution and solvent you will pull more plant fats/oils which we dont want. Most solutes dissolve better in warm/hot solvents, warmer solvent = more saturated pull.

Thanks for that Th Entity I'll heat my solvent and pull at room temp

 

[Th Entity]

No problem, you can share results if you want (you dont have to)
Keep your basic/rootbark solution at room temp and heat solvent(heat bath) untill warm to touch and then start pulling.

 

[pete666]

Every coin has two sides, everything has pros and cons.
There may be two aims in simple extraction without additional purification - high purity or high gain. The first calls for many shorter pulls by more selective solvent (naptha or even heptane), the latter for few long heated pulls with less selective solvent (toluene, xylene)

If you are after high gain and high purity within one extraction, I suggest initial extraction by toluene/xylene and then mini-A/B with heptane re-X. This will result in two fractions - white and orange. Both are very potent though. This strategy assures you get the most out of the bark.

Second strategy might be doing first pulls by cold naptha and latter pulls with heated naptha. Separate precipitation yields vairous products.

 

[Ulim]

Second strategy might be doing first pulls by cold naptha and latter pulls with heated naptha. Separate precipitation yields vairous products.

I fully recommend this.
Low purity dmt can be bad for many ROA like vaporizers or eliquid so i recommend to make different "fractions" and not mixing the dmt.
Lower purity dmt is not useless though since you can still use it for stuff like pharmhuasca or you can simply collect it for a recrystillisation.

I simply do the pull, freeze it, then pour the naptha back into the extraction without the dmt. Then while the solvent is left to soak in the base soup again. I leave the dish to dry and harvest.

This way you save on solvent and you get the highest purity you can get.
Im using light naptha I cleaned through distillation. Its bp 60-95c C6-C7 branched and unbranched (cyclohexane) hydrogenated naptha. (benzene free)

I wouldnt recommend ever to combine many pulls into one simply because you "ruin" the quality by averaging out the purity.

I rather have really pure dmt and some impure instead of dmt that is "meh"

 

[pete666]

Sorry, there was a mistake in my previous post. It has been corrected.

 

[Brennendes Wasser]

I did not read all the answers, so maybe this is not interesting or new: But I just want to tell you the best way IMO


Heat the soup (!) and heat it as high as your solvent starts to boil.

Then throw your pulling solvent into the soup.

Indeed mixing both will equilibrate the temperature inbetween, but there is 1 important thing:


Your pulling solvent will definetly have a lower Heat Capacity (than the water aka the soup) - meaning that it gets warmed up much faster in comparison to water.

This means FOR EXAMPLE

1 L Water (60 °C) + 1 L Hexane (20 °C) will not be at 40 °C, but somewhere 50 - 60 °C.

But if you just heat your soup to the vaporisation temp of the pulling solvent, then you will not come out on a higher temp, so you dont have to fear that it will instantly start vaporizing like hell upon combining.

Ok so this for the pre-heating ...

Then I would advise to slowly heat up until you actually reach that evaporation temp of the solvent and try to let it stay at this point or just below it.

If you plan on letting it stirr together for a long time like 5 minutes or even 10, then you should stay some degrees below that vaporisation temp however.




And for that question: Heat it at all, or not heat it at all -> I would say ALWAYS heat it and ALWAYS heat it to the maximum of your solvent.

You should recrystallize it after you're done anyways, so that little more impurities are totally not bad, as you will get rid of them anyways.

Don't worry: *Recrystallizing* seems to be another thing on top of your route and you may think "ugh ... do I really have to make even more efforts?"

But it is really fast, you will see and so easy. People say: You will loose some of your product. But in my opinion you simply loose the impurities, therefore of course it gets lighter. But it is always worth it! Just make sure that you freeze-precip it fully, then you wont loose any noticable amount of your actives. Plus even when *not focussing on purity* by heating while pulling, after the recrystallization your product will still be like 95 % pure or higher, easily, if done right. Therefore its no real choice between purity and yield.


Let's take a look why I would highly advise it doing it that way (numbers are just examples):

A.) No Heating: You will need 6 pulls to get everything out, which could be 6 x 100 = 600 ml

B.) Heating at max: You will need 3 pulls to get everything out, which could be 3 x 100 = 300 ml

Then you will recrystallize afterwards anyways. You will need lets say 100 ml.

A.) = 6 x 100 + 100 = 700 ml

B.) = 3 x 100 + 100 = 400 ml

Just a rough example, but it is like this. Also you dont know if room temperature will EVER get even the last bit out, maybe even the 6th pull is missing some little amount.

 

[sbc1]

I did not read all the answers, so maybe this is not interesting or new: But I just want to tell you the best way IMO


Heat the soup (!) and heat it as high as your solvent starts to boil.

Then throw your pulling solvent into the soup.

Indeed mixing both will equilibrate the temperature inbetween, but there is 1 important thing:


Your pulling solvent will definetly have a lower Heat Capacity (than the water aka the soup) - meaning that it gets warmed up much faster in comparison to water.

This means FOR EXAMPLE

1 L Water (60 °C) + 1 L Hexane (20 °C) will not be at 40 °C, but somewhere 50 - 60 °C.

But if you just heat your soup to the vaporisation temp of the pulling solvent, then you will not come out on a higher temp, so you dont have to fear that it will instantly start vaporizing like hell upon combining.

Ok so this for the pre-heating ...

Then I would advise to slowly heat up until you actually reach that evaporation temp of the solvent and try to let it stay at this point or just below it.

If you plan on letting it stirr together for a long time like 5 minutes or even 10, then you should stay some degrees below that vaporisation temp however.




And for that question: Heat it at all, or not heat it at all -> I would say ALWAYS heat it and ALWAYS heat it to the maximum of your solvent.

You should recrystallize it after you're done anyways, so that little more impurities are totally not bad, as you will get rid of them anyways.

Don't worry: *Recrystallizing* seems to be another thing on top of your route and you may think "ugh ... do I really have to make even more efforts?"

But it is really fast, you will see and so easy. People say: You will loose some of your product. But in my opinion you simply loose the impurities, therefore of course it gets lighter. But it is always worth it! Just make sure that you freeze-precip it fully, then you wont loose any noticable amount of your actives. Plus even when *not focussing on purity* by heating while pulling, after the recrystallization your product will still be like 95 % pure or higher, easily, if done right. Therefore its no real choice between purity and yield.


Let's take a look why I would highly advise it doing it that way (numbers are just examples):

A.) No Heating: You will need 6 pulls to get everything out, which could be 6 x 100 = 600 ml

B.) Heating at max: You will need 3 pulls to get everything out, which could be 3 x 100 = 300 ml

Then you will recrystallize afterwards anyways. You will need lets say 100 ml.

A.) = 6 x 100 + 100 = 700 ml

B.) = 3 x 100 + 100 = 400 ml

Just a rough example, but it is like this. Also you dont know if room temperature will EVER get even the last bit out, maybe even the 6th pull is missing some little amount.

Thanks Brennendes Wasser but what about just keeping the soup at room temp and heating the solvent to just under its boiling point won't that do the same job if you mix it quickly, that's what I've been doing and every pull has been snow white and I've not had to re-x. The only the problem I face is I don't know how many pulls are needed at room temp

 

[Brennendes Wasser]

Well the pulls are snow white, as your mixture of both will not be really warm, causing not much impurities to get pulled also. As this is a good point on one hand, it may still be the fact on the other as I mentioned, that you MAAAYYY need much more pulls than neccessary.


Why I think your way is not a good option, if you want to pull at the highest temperature - but only IF you want to pull at the highest temperature, which I always recommend:



You have 500 ml of H2O-Soup at 20 °C

You have 100 ml of Pulling-Solvent at 60 °C


Now you mix your 500 ml H2O (20 °C) + 100 ml Naphtha (60 °C) and this will surely be somewhere like

20 - 25 °C in temperature.

1. You have much more water, but even more important

2. Water has a much higher heat capacity 4,12 kJ/kg*K
= to heat 1 kg of water by 1 K or °C you need 4,12 kJ

than Hexane (I take this as Naphtha) with 2,30 kJ/kg*K
= to heat 1 kg of hexane by 1 K or °C you need 2,30 kJ

This means that a 50:50 Mixture of Water and Hexane will already be at 2/3 of the temperature towards water. And a mixture of 500:100 ml will be nearly only as warm as the water itself.


By this calculation you see that you should always pull nearly with room temp, when you do it that way AND if you also use those volumes.
If you have 500 ml Soup and 500 ml Nephtha and you have 20 and 60 °C, then it will be like 30 °C.

Still pretty low. But if you can control the temperature of the soup, then I guess you can also just check the temperature of the mixture when you threw it together? You should just make a quick check the next time.

Yes - pulling at low temperature gives the purest crystals.

But to check if you are missing some yield because of that low temperature or if you need toooo many pulls to get the maximum, then you know yourself, that you COULD heat it more and make less pulls with a recrystallization.



Let's say it like this:

In my case I have that experience, considering Yield with max heating:


1. Pull at max. Temp = 80 %

2. Pull at max. Temp = 17 %

3. Pull at max. Temp = 3 % or less

A 4. Pull is not necessary at the max Temperature. And IMO a 1:0,2 ratio of Water-soup to Pulling agent is good, so for 1 L this would be 3 x 200 ml of pulling agent.
I see people do 5 or more pulls, but with max temperature even the 3. one will nearly already be not worth it and just to be sure to get everything out.

Check your own numbers then you can see if you should change something, or if its already pleasant for you = ) :thumb_up:

 

[sbc1]

Well the pulls are snow white, as your mixture of both will not be really warm, causing not much impurities to get pulled also. As this is a good point on one hand, it may still be the fact on the other as I mentioned, that you MAAAYYY need much more pulls than neccessary.


Why I think your way is not a good option, if you want to pull at the highest temperature - but only IF you want to pull at the highest temperature, which I always recommend:



You have 500 ml of H2O-Soup at 20 °C

You have 100 ml of Pulling-Solvent at 60 °C


Now you mix your 500 ml H2O (20 °C) + 100 ml Naphtha (60 °C) and this will surely be somewhere like

20 - 25 °C in temperature.

1. You have much more water, but even more important

2. Water has a much higher heat capacity 4,12 kJ/kg*K
= to heat 1 kg of water by 1 K or °C you need 4,12 kJ

than Hexane (I take this as Naphtha) with 2,30 kJ/kg*K
= to heat 1 kg of hexane by 1 K or °C you need 2,30 kJ

This means that a 50:50 Mixture of Water and Hexane will already be at 2/3 of the temperature towards water. And a mixture of 500:100 ml will be nearly only as warm as the water itself.


By this calculation you see that you should always pull nearly with room temp, when you do it that way AND if you also use those volumes.
If you have 500 ml Soup and 500 ml Nephtha and you have 20 and 60 °C, then it will be like 30 °C.

Still pretty low. But if you can control the temperature of the soup, then I guess you can also just check the temperature of the mixture when you threw it together? You should just make a quick check the next time.

Yes - pulling at low temperature gives the purest crystals.

But to check if you are missing some yield because of that low temperature or if you need toooo many pulls to get the maximum, then you know yourself, that you COULD heat it more and make less pulls with a recrystallization.



Let's say it like this:

In my case I have that experience, considering Yield with max heating:


1. Pull at max. Temp = 80 %

2. Pull at max. Temp = 17 %

3. Pull at max. Temp = 3 % or less

A 4. Pull is not necessary at the max Temperature. And IMO a 1:0,2 ratio of Water-soup to Pulling agent is good, so for 1 L this would be 3 x 200 ml of pulling agent.
I see people do 5 or more pulls, but with max temperature even the 3. one will nearly already be not worth it and just to be sure to get everything out.

Check your own numbers then you can see if you should change something, or if its already pleasant for you = ) :thumb_up:

I'm currently doing 1 - 3kg extractions so my vessel's vary from 5l to 10l depending on the extraction, and depending wheather I do everything in the bottle or an acid cook and strain first, so at the moment I'm using a 5l bottle and usually pulling with 200-300ml hot solvent to room temp soup.

 

[Brennendes Wasser]

Ok but in this case you wont need to heat your solvent anyways, as it will be instantly at room temperature upon the mixture with your soup.

Sadly the solubility of your goodies is pretty low at room temperature ...

Do you already have any results?

If the yield is very low, then this was probably the problem.

Also: That is a fairly huge amount, I know its easier to do just 1 big extraction instead of 5 tiny ones, but it also makes the whole process a little bit more complicated and harder to fix problems.

To make it easier, you could reduce it further. Then you can also heat up the soup more easily.

If everything works out the way you are doing, you should still only get a very tiny amount of yield each pull as the volume of Soup is still really high and your pulling solvent will not be warm at all while extracting.

So if you're not already done, then check the yield and if it is pretty low, then this may be a point to improve.

Also big extractions tend to be a little less effective, as you will always loose more inbetween steps, so maybe a 3 kg extraction will not grant you 30 g Spice, but more likely 25 or even only 20. That may also be a point to consider, if you think your yield is kind of low.

 

[some one]

1 - 3kg extractions, wow :surprised

@ Brennendes Wasser:

1. Pull at max. Temp = 80 %
2. Pull at max. Temp = 17 %
3. Pull at max. Temp = 3 % or less

Did you measure this result or are your giving an arbitrary example?

Just wondering, how much dirty spice do you put in how much Naphtha for re-x? 1g per 50ml? I guess it doesn't matter much if the spice is, say, 2x as dirty from 60 C pulls then from 40 C pulls, as in, there being less actual spice per 1g to re-x.

 

[Brennendes Wasser]

Yoo this was indeed something which I measured O:

I dont completely understand this

Just wondering, how much dirty spice do you put in how much Naphtha for re-x? 1g per 50ml? I guess it doesn't matter much if the spice is, say, 2x as dirty from 60 C pulls then from 40 C pulls, as in, there being less actual spice per 1g to re-x.

xD

But it was somehow like this:

The process was somehow like this, calculated upwards to 1 kg bark

1 kg was cooked 2x with 4 L per kg bark

then all L were combined and reduced to 1 L per Bark (this is a pretty high concentration in the end - therefore I guess it is that high yield within the very first pulls).

Then all 3 pulls were done with 1:5 Naphtha:Water, but with Hexane/Pentane-Naphtha (40/60°C), and not with Hexane/Heptane-Naphtha (60/80°C).

This way it is already pure enough for the direct usage.



BUT

I have a new result where I did not concentrate the soup that hard and this time there was still something to be pulled out when I additionally threw 60/80°C on it, after I did the 3 pulls with 40/60°C. Therefore either its not really repeatable or the three pulls that gave everything mostly relied on the hyper concentrated soup. Don't know, but I will soon start some tests about solubility in 40/60 + 60/80 and also how the pulling process is when you pull X g out of 1 L and X g out of 2 L in terms of efficiency ... ;O

 

[sbc1]

1 or 2 shouldn't matter though should it as all the dmt is there anyway, with more water it's easier for the naphtha to seperate as it's not to thick

 

[Brennendes Wasser]

Well in general this could be a good point, but IMO if you totally (!) filtered your acidic Soup then the volume totally does not matter.

No separation between layers is often if the acidic soup is not totally free of tiny particles. After filtering through a half of a cotton shirt (and squeezing it out to get liquid out of it) you will be left with a solution which will separate from Naphtha at any concentration level (ok of course you need to filter again, if you concentrate further after filtration process).

 

[sbc1]

I do 3 filtrations so I'm left with hardly any particles but I what I ment was that with 1l of acidic mix or 5l of acidic mix it won't matter because all the dmt the bark has give will be there, it's just down to wheather you want to work with 1l or 5l

 

[some one]

I dont completely understand this: "Quote: Just wondering, how much dirty spice do you put in how much Naphtha for re-x? 1g per 50ml? I guess it doesn't matter much if the spice is, say, 2x as dirty from 60 C pulls then from 40 C pulls, as in, there being less actual spice per 1g to re-x."

I meant that I use 50ml Naphtha per 1g spice to re-x. But if the spice has a high impurity due to super high temp pulls, then 1g yield might only contain 600mg spice and 400mg inactives. Using 50ml naphtha for 600mg spice might be too much naphtha, which leads to a relatively less pure after re-x yield. But I haven't tested this so it might not be a big problem in practice.

Anywayz. I did a new cyb tek extraction and tested the high temp pull method.

Procedure:

Batch #1: 50g MHBR. Acidify @ 20 C. Base @ 20 C. Pull @ 20 C (freeze/thaw during acid)
Batch #2: 50g MHBR. Acidify @ 70 C. Base @ 60 C. Pull @ 20 C (no freeze)
Batch #3: 50g MHBR. Acidify @ 70 C. Base @ 60 C. Pull @ 35 C (no freeze)
Batch #4: 50g MHBR. Acidify @ 70 C. Base @ 60 C. Pull @ 60 C (no freeze)

Results:

Batch #1 freeze: pull 1-3 0mg    pull 4 28mg  pull 5 30mg  total 58mg
Batch #2 cold:   pull 1-3 0mg    pull 4 20mg  pull 5 34mg  total 54mg
Batch #3 warm:   pull 1-3 218mg  pull 4 34mg  pull 5 54mg  total 287mg (0.6%)
Batch #4 hot:    pull 1-3 725mg  pull 4 0mg   pull 5 0mg   total 725mg (1.5%)

Observations:

- I gradually decreased the NPS pull volume from 75ml (first pulls) to 50ml (last pulls). This might explain why batch #1 and #2 had no yield in the first 3 pulls. Maybe the specific naphtha brand type was too little saturated to precip DMT at lower concentrations? I will evap the naphtha down to 30% and freeze precip again. Will share results.

- Seems like freeze/thaw during acid stage has the same effect on yield as heating the acid and base stage without freeze/thaw.

- DMT yield was 100% white for batch #1 (freeze). Clean for batch #2 (cold). Dark spots for pulls 1-3 of batch #3 (warm) and oily yellow with dark orange and brown for batch #4 (hot).

- relatively (neglectable) low yield impurities arise from heating during acid and base. The impurities are mostly pull temp related.

- Batch 4 was very oily. I will re-x and share the final weight. Expect it to be around 1%.

Conclusions:

- Seems like blasting 60 C hot pulls gets all the actives out in 3 pulls. I will do 2 additional 60 C pulls on batches 1-3 to get all actives out from these.

- Felt a bit light headed after the extraction. Ventilation and mask did not seem to be sufficient to protect again the hot naphtha fumes. These can escape from jar like large sized screw-on bottle lids. Make sure to have really good ventilation when heating solvents!

 

[Brennendes Wasser]

Nice results ! ;O

Yeah seems like there is totally NO REASON to pull cold.

I mean yes, less impurities. But you will get away of them anyways. And if 1 re-x does not satisfy, then the next one can be done nevertheless.

Just one question to understand your other temperatures:

Acidify @ 20 C -> this means you did the acidic cook of the bark in 20 °C?

Pull @ 20 C -> this means you extracted with Naphtha at 20 °C?

Ok this is clear but what means:

Base @ 60 C --> ;O ?


I am also doing some tests to find out how one TEK could be improved, like how the volume of the soup compared to the NPS should be - to check when its the perfect place to stop reducing before pulling. Also what the effect on salting would be.

So far I have the feeling that salting the soup does not push any Spice further into the Naphtha. Maybe it COULD help separating layers, but this was never a problem so far. Lastly one time excessive salting made a lot of stuff crash out, which ruined the separation process :thumb_dow And some other stuff is in my mind, maybe I can share this within the next weeks.

I was using PENTAN/Hexane-Naphtha as it produces already like 98 % + purity, but the last try did not get everything out within the first 3 pulls, so maybe I need to check solubility of plain Spice in both and compare. Maybe good-old Hexane/Heptan-Naphtha would still be better then ...

 

[sbc1]

Nice results ! ;O

Yeah seems like there is totally NO REASON to pull cold.

I mean yes, less impurities. But you will get away of them anyways. And if 1 re-x does not satisfy, then the next one can be done nevertheless.

Just one question to understand your other temperatures:

Acidify @ 20 C -> this means you did the acidic cook of the bark in 20 °C?

Pull @ 20 C -> this means you extracted with Naphtha at 20 °C?

Ok this is clear but what means:

Base @ 60 C --> ;O ?


I am also doing some tests to find out how one TEK could be improved, like how the volume of the soup compared to the NPS should be - to check when its the perfect place to stop reducing before pulling. Also what the effect on salting would be.

So far I have the feeling that salting the soup does not push any Spice further into the Naphtha. Maybe it COULD help separating layers, but this was never a problem so far. Lastly one time excessive salting made a lot of stuff crash out, which ruined the separation process :thumb_dow And some other stuff is in my mind, maybe I can share this within the next weeks.

I was using PENTAN/Hexane-Naphtha as it produces already like 98 % + purity, but the last try did not get everything out within the first 3 pulls, so maybe I need to check solubility of plain Spice in both and compare. Maybe good-old Hexane/Heptan-Naphtha would still be better then ...

Base was heated to 60 then added his naphtha which was 60