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Brennendes Wasser
Chemical expert
#21 Posted : 2/13/2019 5:29:29 PM
Oh of course ... hehe

But again everyone should JUST heat the soup, as the Naphtha will equilibrate nearly at the temperature of the soup upon combining, it takes nearly no heat to get up to that temperature. Now you can do what you want, but why heat 2 soups separately, when you could just heat 1 and you will get the same results?

I will just calculate it here, those are the heat capacities:

0,19497 J/(mol·K) (25 °C) for Hexan

and

4,184 J/(kg·K) (14,5 °C) for water

Ok it changes with temperature and Naphtha is not just hexan so its not 100% accurate, but I guess you get the point:

Ok we have 1 L of water and we throw in 200 ml of Napthha.
First let's check how much heat we applied to the water to raise it to 60 °C:

delta Q = m * cp * delta T
= 1 kg * 4,184 kJ/kgK * 40 K = 167,4 kJ

and now how much heat is needed to get 200 ml Naphtha up to that temperature? Weight of Naphtha: 200 ml and it wieghs 660 g per Liter = 0,2*660 = 132 g and this is 1,53 mol.

delta Q = 1,53 mol * 0,19497 J/molK * 40 K
= 11,9 kJ

This means the Naphtha will steal like 12 kJ out of 167,4 kJ from the water, leaving the water at ~ 57 °C.

Therefore to be 100 %ly safe, just heat the water to 63 °C and throw your Naphtha in, it should be 60 °C Very happy

Of course all those stuff dissolved in the water would raise the needed heat a bit, but if so then don't heat it to 63 but to 65 or whatever, also simply trying it out instead of Math would make it clear.

long story short I just want to show everyone that

A: heating Naphtha is a waste of time when you could just add 3 more °C for your soup

B: heating Naphtha and NOT HEATING the soup is totally pointless, you will end up at 20 °C in the end anyways, as if you did not heat anything at all.



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


I dont completely understand the freeze - thaw, so this means that AFTER you did the acidic cook you froze and thawed the soup?
Normally I thought it was recommended to do this before the actual cooking step. Is there a benefit to do it with the soup? If I get it correctly you use it before basifying, but then you already dismissed the plant material and I thought the freeze-thaw is to break it upen prior to the acidic extraction step.

Also in that quote you say possibly it has the same effect.

But it may also be that (if I got it correctly and you did it AFTER you already dismissed the plant amterial) it has no effect. You have nearly the same yield like with the 60 °C base + 20 °C soup.

But 60 °C + 20 °C soup should be like 22 - 23 °C overall. So this would be nearly as no temperature increase at all. Therefore one may say that this is just 20 °C of both and NO freeze-thaw step.
And as the freeze-thaw test had the same result like this, it seems like the freeze-thaw did not make any difference.

So I understood that you did the freeze-thaw AFTER the initial cook, but maybe I got you wrong and you mean before.
And then this would be really interesting, as all people tell to do one before cooking and your test is basically:

Freeze-Thaw vs. no Freeze-Thaw

And it does not seem like the freezing did improve the yield at all.

I also wanted to do a test on this, but haven't done so far as it is just so easy to freeze-thaw as you do not need to do anything meanwhile. But I am also really curious is this REALLY improves anything or not. Because we should definetly check it out, as everyone tells it and everyone does it and probably it is not even needed?

I could only imagine if you just cook your stuff for 10 mins, then maybe it makes a difference, but who is only cooking for 10 mins ? Oô
 
some one
#22 Posted : 2/14/2019 8:57:35 AM
I think you're misunderstanding me Smile

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)

Acidify @ 20 C: I added an acidic solution with pH 3-4 to dry coffee grind sized MHRB. 20 C means I didn't heat the solution, but left it at room temp (around 20 C). 70 C means I heated the entire solution to 70 C.

Freeze/thaw during acid: After adding the acidic solution to the bark I placed the solution with the bark in the freezer for the night. The acidic solution already soaked the bark, but freezing will have the water molecules expand when they change to ice, cracking (fracking) the parts of the bark which are still a bit solid. My observations showed that this has the same effect on yield than heating the acidic and base stages. Meaning, you could choose not to heat, to save energy. But to be sure I need to do a comparison between freezing vs heated acid and base stages with a hot pull stage (only did cold pulls for this comparison now).

Base @ 60 C: This is the temp of the entire solution during the basing stage. With basing I mean increasing the pH > 12 (adding lye). This is the soup.

Pull @ 60 C: This is the temp of the entire solution during the pulling stage (adding NPS). No, I didn't preheat the naphtha on its own. I advice against this. First of all what you say about temp flow is right. Second you want to minimize petrochemical NPS fume exposure. Preheating NPS and pouring from one container into the next causes more fumes in your work area.

Quote:
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 Thumbs down And some other stuff is in my mind, maybe I can share this within the next weeks.

Yes, please do. We can always use more AB tests (comparison tests).
some = one | here = some | there = one
 
Brennendes Wasser
Chemical expert
#23 Posted : 2/14/2019 11:40:56 AM
Quote:
No, I didn't preheat the naphtha on its own. I advice against this.


No worries! I wrote that whole calculation stuff not because of you, but because of the Thread Creator who only heated his NPS and not the soup. And of course for all others that may do it like this.

Ok good to know what you mean with that Base @ X Number =)

But one question: Do you really think that it matters at what temperature the Soup is while getting from pH ~ 3 to pH ~ 12 ?

I mean ... in this stage you do not dissolve something out of anything so a higher temperature does not seem to make any difference for me at this stage ; O

So the reason is to freebase your Goodies and they will get freebased even on 5 °C - as pH ~ 12 always means that everything is deprotonated.



And second: Yes it really looks like that freeze/thaw got the same yield as heating it while cooking then. But I really would test this out one more time, because doesnt this sound a bit strange? I mean everyone says to freeze/thaw and then ALSO cook it hot. It would be strange that the freezing thing could totally replace it.

Of course you say it is to make the cells burst which should (in theory) help to dissolve all goddies in the water. But still at low temperatures I would just think that the dissolvation process is very slow at all, even if the cells bursted before or not. So I would really think that hot acidic cook should be worth it always, as heat is a factor to dissolve something for everything : S



I mean it could be like this:

You did those 2 tests to compare it with 20 °C pulls. Let's say at 20 °C the dissolvation power of Naphtha is only like 10 % of the total Spice in contrast to maybe 30 % when hot.

Then when you did that 20 °C test with freeze/thaw you did not dissolve much out of the bark, as it was not heated (let's just say it like this for this mind experiment). Let's say you only dissolved 50 % of every goodies out of the bark.

Then you did the hot acidic cook at 70 °C. Here you got 100 % out of the bark.

But now you pull at 20 °C and we say that cold Naphtha can only hold like 10 % of all DMT in one pull.

Then when you do 5 pulls on the Batch #1, you will get 5 x 10 % = 50 % of Spice. Got everything out.

Then when you do 5 pulls on the Batch #2, you will get 5 x 10 % = 50 % of Spice. But there is still 50 % in there, which you did not get as the solvent was too cold.

Now you would assume that both TEKs were equally nice as you got the same results - low yield, but the same yield.



So I guess IF this mind experiment would be correct, then this may be the reason why Batch #1 and Batch #2 gave the same results. Therefore it should definetly be done with heating the solvent to the max to check if ONLY freeze/thaw indeed is equals a real acidic cook.


Long Post, sorry Rolling eyes :

But from another Test which I did for the optimization I am already pretty sure that additional cooking MUST enlarge the yield. This bark was also Frozen/thawed, so it involved both.

I did a test on how much was dissolved after what time.

I did 2 acidic cooks in a row and checked every 30 minutes the content of it.

The results will be packed in a nice chart, therefore I will only give the numbers here, but I guess they already tell something to this point:

Acidic Cook pH = 3, 80 °C

t = 10 min (still 20 °C) -> 46 %

t = 30 min (now at 80 °C) -> 65 %

t = 60 min -> 77 %

t = 120 min -> 82 %

[now the water is exchanged with new water]

t = 180 min -> 89 %

t = 240 min -> 100 %

I dont know if at 240 min = 100 %, but this is when I stopped and I think the bark should be nearly exhausted.

So based on this I would state that without heating and only with freeze/thaw I would only have gotten that first 46 % when I unfroze it. It seems like a lot of goodies come into the water at low temperatures, but to get everything out you need heat.

This is my result but I would really think it is reproducable.

Maybe you could indeed do this test with no acidic cook, but hot pulling to check your results, but it would be very uncommon that no heat is needed to get everything out Shocked

Best regards
 
some one
#24 Posted : 4/14/2019 2:41:29 PM
Quote:
Do you really think that it matters at what temperature the Soup is while getting from pH ~ 3 to pH ~ 12? I mean ... in this stage you do not dissolve something out of anything so a higher temperature does not seem to make any difference for me at this stage. So the reason is to freebase your Goodies and they will get freebased even on 5 °C - as pH ~ 12 always means that everything is deprotonated.

Basing temp doesn't matter if the bark is discarded after multiple acid cooks. But when keeping the bark in same solution Cyb style (one acid cook), the acid doesn't take all actives out which continue to to come out during the basing stage. Basing at higher temp means more actives come out into the solution.

Quote:
Yes it really looks like that freeze/thaw got the same yield as heating it while cooking then. But I really would test this out one more time, because doesnt this sound a bit strange? I mean everyone says to freeze/thaw and then ALSO cook it hot. It would be strange that the freezing thing could totally replace it.

This was just a test to see what happens with room temp for the entire procedure. I could have also chosen not to freeze/thaw this batch for less variables.

Quote:
Of course you say it is to make the cells burst which should (in theory) help to dissolve all goddies in the water. But still at low temperatures I would just think that the dissolvation process is very slow at all, even if the cells bursted before or not. So I would really think that hot acidic cook should be worth it always, as heat is a factor to dissolve something for everything

Yes always use higher temp for the acid cook.

Quote:
[...] So I guess IF this mind experiment would be correct, then this may be the reason why Batch #1 and Batch #2 gave the same results. Therefore it should definetly be done with heating the solvent to the max to check if ONLY freeze/thaw indeed is equals a real acidic cook.

Yes for completeness an extra test would be needed: hot pulls on cold acid/base. But you shouldn't acid/base cold anyway.

Quote:
t = 10 min (still 20 °C) -> 46 %
t = 30 min (now at 80 °C) -> 65 %
t = 60 min -> 77 %
t = 120 min -> 82 %
t = 180 min -> 89 %
t = 240 min -> 100 %

The percentage is the amount of DMT obtained from extracting vs the total amount of DMT present in the bark? Meaning a 60 min acid cook at 80 C on 100g bark containing 1% DMT yields 0.77g? How did you perform this experiment?
some = one | here = some | there = one
 
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